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_2108099
_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         'C14 H7 N2 Ni O8, H3 O, H2 O, O'
_chemical_formula_sum            'C14 H12 N2 Ni O11'
_chemical_formula_weight         442.97
_chemical_name_systematic        '[Ni(pydcH)(pydc)](H3O)(H2O)2]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_atom_sites_solution_secondary   difmap
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_cell_formula_units_Z            4
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_cell_length_b                   10.0554(6)
_cell_length_c                   13.7813(8)
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_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa DUO with Photon 100 detector'
_diffrn_measurement_method       '\w and \f'
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_diffrn_reflns_theta_max         31.580
_diffrn_reflns_theta_min         2.602
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Shedrick, 2014)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.340
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.726
_refine_ls_extinction_coef       0.0236(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5701
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0564P)^2^+0.8461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1102
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_reflns_number_total             5701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb5059sup1.cif
_cod_data_source_block           298d
_cod_database_code               2108099
_shelx_estimated_absorpt_t_min   0.603
_shelx_estimated_absorpt_t_max   0.686
_shelx_hkl_checksum              76692
_shelx_res_checksum              83780
_cod_database_fobs_code 2108099