An ordering phase transition, short hydrogen bonds and high <i>Z</i>' in the structure of Ni(Hpydc)~2~·3H~2~O
Derikvand, Zohreh; Powers, Xian B.; Olmstead, Marilyn M.; Acta Crystallographica Section B 73 (2017) 413–418; doi:10.1107/S2052520617004334

data_2108098
_publ_section_title
;
 An ordering phase transition, short hydrogen bonds and high <i>Z</i>' in
 the structure of Ni(Hpydc)~2~&#x00B7;3H~2~O
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              413
_journal_page_last               418
_journal_paper_doi               10.1107/S2052520617004334
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety
'3(C14 H6 N2 Ni O8), C14 H8 N2 Ni O8, 3(H3 O), 4(H2 O), H O, 4(O)'
_chemical_formula_sum            'C56 H44 N8 Ni4 O44'
_chemical_formula_weight         1767.75
_chemical_name_systematic        '[Ni(pydcH)2](H2O)3'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 115.261(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5303(18)
_cell_length_b                   19.6477(13)
_cell_length_c                   13.7534(9)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.65
_cell_volume                     6727.9(8)
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_collection       'Apex 3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS (Shedldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa DUO with Photon 100 detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         2.360
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.340
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.716
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         14609
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+29.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                13325
_reflns_number_total             14609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb5059sup1.cif
_cod_data_source_block           180c
_cod_database_code               2108098
_shelx_estimated_absorpt_t_min   0.598
_shelx_estimated_absorpt_t_max   0.682
_shelx_hkl_checksum              81928
_shelx_res_checksum              49878
_cod_database_fobs_code 2108098