Multiple-Step Humidity-Induced Single-Crystal to Single-Crystal Transformations of a Cobalt Phosphonate: Structural and Proton Conductivity Studies.
Cai, Zhong-Sheng; Bao, Song-Song; Wang, Xi-Zhang; Hu, Zheng; Zheng, Li-Min; Inorganic chemistry 55 (2016) 3706–3712; doi:10.1021/acs.inorgchem.6b00413

data_4347638
_publ_section_title
;
 Multiple-Step Humidity-Induced Single-Crystal to Single-Crystal
 Transformations of a Cobalt Phosphonate: Structural and Proton
 Conductivity Studies.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3706
_journal_page_last               3712
_journal_paper_doi               10.1021/acs.inorgchem.6b00413
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '2(C9 H19 Co N O8 P2), H2 O'
_chemical_formula_sum            'C18 H40 Co2 N2 O17 P4'
_chemical_formula_weight         798.26
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 114.182(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.261(5)
_cell_length_b                   6.2566(19)
_cell_length_c                   15.639(5)
_cell_measurement_reflns_used    2358
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.034
_cell_measurement_theta_min      2.351
_cell_volume                     1451.5(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6933
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.613
_exptl_absorpt_coefficient_mu    1.445
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.696
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1280P)^2^+25.8104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2486
_refine_ls_wR_factor_ref         0.2666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2049
_reflns_number_total             2749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00413_si_004.cif
_cod_data_source_block           3
_cod_original_cell_volume        1451.5(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347638
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2013-4
_shelx_res_checksum              679
_shelx_hkl_checksum              50359