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Na2NiCPO7 crystallizes in the triclinic P1 space group. The structure is three-dimensional. there are eight inequivalent Na1+ sites. In the first Na1+ site, Na1+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Na–O bond distances ranging from 2.34–2.84 Å. In the second Na1+ site, Na1+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Na–O bond distances ranging from 2.33–2.96 Å. In the third Na1+ site, Na1+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Na–O bond distances ranging from 2.28–2.78 Å. In the fourth Na1+ site, Na1+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Na–O bond distances ranging from 2.33–2.77 Å. In the fifth Na1+ site, Na1+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Na–O bond distances ranging from 2.32–2.85 Å. In the sixth Na1+ site, Na1+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Na–O bond distances ranging from 2.31–3.00 Å. In the seventh Na1+ site, Na1+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Na–O bond distances ranging from 2.32–2.97 Å. In the eighth Na1+ site, Na1+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Na–O bond distances ranging from 2.31–2.78 Å. There are four inequivalent Ni3+ sites. In the first Ni3+ site, Ni3+ is bonded to six O2- atoms to form distorted NiO6 octahedra that share corners with four PO4 tetrahedra. There are a spread of Ni–O bond distances ranging from 1.97–2.19 Å. In the second Ni3+ site, Ni3+ is bonded to six O2- atoms to form NiO6 octahedra that share corners with four PO4 tetrahedra. There are a spread of Ni–O bond distances ranging from 2.00–2.12 Å. In the third Ni3+ site, Ni3+ is bonded to six O2- atoms to form NiO6 octahedra that share corners with four PO4 tetrahedra. There are a spread of Ni–O bond distances ranging from 1.98–2.10 Å. In the fourth Ni3+ site, Ni3+ is bonded to six O2- atoms to form NiO6 octahedra that share corners with four PO4 tetrahedra. There are a spread of Ni–O bond distances ranging from 1.98–2.12 Å. There are four inequivalent C4+ sites. In the first C4+ site, C4+ is bonded in a trigonal planar geometry to three O2- atoms. There are a spread of C–O bond distances ranging from 1.27–1.31 Å. In the second C4+ site, C4+ is bonded in a trigonal planar geometry to three O2- atoms. There is one shorter (1.26 Å) and two longer (1.30 Å) C–O bond length. In the third C4+ site, C4+ is bonded in a trigonal planar geometry to three O2- atoms. There is one shorter (1.25 Å) and two longer (1.31 Å) C–O bond length. In the fourth C4+ site, C4+ is bonded in a trigonal planar geometry to three O2- atoms. There are a spread of C–O bond distances ranging from 1.26–1.31 Å. There are four inequivalent P5+ sites. In the first P5+ site, P5+ is bonded to four O2- atoms to form PO4 tetrahedra that share corners with four NiO6 octahedra. The corner-sharing octahedra tilt angles range from 40–47°. There are a spread of P–O bond distances ranging from 1.54–1.56 Å. In the second P5+ site, P5+ is bonded to four O2- atoms to form PO4 tetrahedra that share corners with four NiO6 octahedra. The corner-sharing octahedra tilt angles range from 40–50°. There are a spread of P–O bond distances ranging from 1.54–1.57 Å. In the third P5+ site, P5+ is bonded to four O2- atoms to form PO4 tetrahedra that share corners with four NiO6 octahedra. The corner-sharing octahedra tilt angles range from 40–50°. There are a spread of P–O bond distances ranging from 1.54–1.57 Å. In the fourth P5+ site, P5+ is bonded to four O2- atoms to form PO4 tetrahedra that share corners with four NiO6 octahedra. The corner-sharing octahedra tilt angles range from 42–49°. There are a spread of P–O bond distances ranging from 1.54–1.57 Å. There are twenty-eight inequivalent O2- sites. In the first O2- site, O2- is bonded in a 3-coordinate geometry to two Na1+ and one C4+ atom. In the second O2- site, O2- is bonded in a 1-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the third O2- site, O2- is bonded in a distorted rectangular see-saw-like geometry to two Na1+, one Ni3+, and one P5+ atom. In the fourth O2- site, O2- is bonded in a 4-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the fifth O2- site, O2- is bonded in a 3-coordinate geometry to one Na1+, one Ni3+, and one P5+ atom. In the sixth O2- site, O2- is bonded in a distorted rectangular see-saw-like geometry to two Na1+, one Ni3+, and one P5+ atom. In the seventh O2- site, O2- is bonded in a 3-coordinate geometry to one Na1+, one Ni3+, and one P5+ atom. In the eighth O2- site, O2- is bonded in a 1-coordinate geometry to three Na1+, one Ni3+, and one P5+ atom. In the ninth O2- site, O2- is bonded in a 4-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the tenth O2- site, O2- is bonded in a distorted trigonal pyramidal geometry to two Na1+, one Ni3+, and one C4+ atom. In the eleventh O2- site, O2- is bonded in a 3-coordinate geometry to one Na1+, one Ni3+, and one C4+ atom. In the twelfth O2- site, O2- is bonded in a 1-coordinate geometry to two Na1+, one Ni3+, and one C4+ atom. In the thirteenth O2- site, O2- is bonded in a 1-coordinate geometry to one Na1+, one Ni3+, and one C4+ atom. In the fourteenth O2- site, O2- is bonded in a 3-coordinate geometry to two Na1+ and one C4+ atom. In the fifteenth O2- site, O2- is bonded in a 3-coordinate geometry to two Na1+ and one C4+ atom. In the sixteenth O2- site, O2- is bonded in a 4-coordinate geometry to two Na1+, one Ni3+, and one C4+ atom. In the seventeenth O2- site, O2- is bonded in a 5-coordinate geometry to three Na1+, one Ni3+, and one C4+ atom. In the eighteenth O2- site, O2- is bonded in a distorted trigonal pyramidal geometry to two Na1+, one Ni3+, and one C4+ atom. In the nineteenth O2- site, O2- is bonded in a 1-coordinate geometry to three Na1+, one Ni3+, and one C4+ atom. In the twentieth O2- site, O2- is bonded in a 1-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the twenty-first O2- site, O2- is bonded in a 1-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the twenty-second O2- site, O2- is bonded in a 1-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the twenty-third O2- site, O2- is bonded in a distorted rectangular see-saw-like geometry to two Na1+, one Ni3+, and one P5+ atom. In the twenty-fourth O2- site, O2- is bonded in a 4-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the twenty-fifth O2- site, O2- is bonded in a 4-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the twenty-sixth O2- site, O2- is bonded in a 3-coordinate geometry to one Na1+, one Ni3+, and one P5+ atom. In the twenty-seventh O2- site, O2- is bonded in a 1-coordinate geometry to two Na1+, one Ni3+, and one P5+ atom. In the twenty-eighth O2- site, O2- is bonded in a distorted rectangular see-saw-like geometry to three Na1+ and one C4+ atom.

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