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_2108097
_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_coeditor_code           EB5059
_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         'C14 H10 N2 Ni O9, 2(H2 O)'
_chemical_formula_sum            'C14 H14 N2 Ni2 O11'
_chemical_formula_weight         444.98
_chemical_name_common            '[Ni(pydcH)(pydc)](H3O)(H2O)2]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                69.7619(11)
_cell_angle_beta                 69.3377(11)
_cell_angle_gamma                69.3655(11)
_cell_formula_units_Z            8
_cell_length_a                   13.7266(12)
_cell_length_b                   16.9157(15)
_cell_length_c                   16.9080(14)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.50
_cell_volume                     3325.9(5)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2015)'
_computing_data_collection       'Apex 2 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2015)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46008
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.261
_diffrn_reflns_theta_min         1.626
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.587
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         16469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.7910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0552
_reflns_number_gt                16170
_reflns_number_total             16469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb5059sup1.cif
_cod_data_source_block           mn2293
_cod_depositor_comments
;

2019-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety
;C14 H12 N2 Ni O10, 2(C14 H10 N2 Ni O9), C14 H7 N2 Ni O8, H3 O,
 7(H2 O)
;
_cod_original_formula_sum        'C56 H56 N8 Ni4 O44'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1779.92
_cod_database_code               2108097
_cod_database_fobs_code          2108097
_shelx_estimated_absorpt_t_min   0.631
_shelx_estimated_absorpt_t_max   0.817
_shelx_hkl_checksum              47079
_shelx_res_checksum              10429