Consistent zincophosphite 4-ring 'ladder' chain structural motif with isomeric ligands.
Wark, Stephen; Lyons, Megan J.; Slawin, Alexandra M. Z.; Harrison, William T. A.; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 272–279; doi:10.1107/S2056989023002062

data_2244228
_publ_section_title
;
 Consistent zincophosphite 4-ring 'ladder' chain structural motif with
 isomeric ligands.
;
_journal_coeditor_code           PK2681
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              272
_journal_page_last               279
_journal_paper_doi               10.1107/S2056989023002062
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '(C6 H9 N2)2 [Zn3 (H P O3)4], H2 O'
_chemical_formula_moiety         '2(C6 H9 N2 +), H4 O12 P4 Zn3 2-, H2 O'
_chemical_formula_sum            'C12 H24 N4 O13 P4 Zn3'
_chemical_formula_weight         752.34
_chemical_name_systematic
;
Poly[bis(2-amino-4-methylpyridinium) [tetra-\m~3~-phosphonato-trizinc]
monohydrate]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                81.03130(10)
_cell_angle_beta                 88.06460(10)
_cell_angle_gamma                80.07820(10)
_cell_formula_units_Z            2
_cell_length_a                   9.03805(13)
_cell_length_b                   9.36837(13)
_cell_length_c                   15.0207(2)
_cell_measurement_reflns_used    10623
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      75.2490
_cell_measurement_theta_min      5.7000
_cell_volume                     1237.46(3)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rigaku Pilatus 200K CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_av_unetI/netI     0.0083
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11869
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.378
_diffrn_reflns_theta_min         2.978
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear (Rigaku, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.668
_refine_ls_extinction_coef       0.0053(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+2.3807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                4831
_reflns_number_total             4842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2681sup1.cif
_cod_data_source_block           IV
_cod_depositor_comments
'Adding full bibliography for 2244225--2244229.cif.'
_cod_database_code               2244228
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.563
_shelx_hkl_checksum              82602
_shelx_res_checksum              349