In situ formed [M(CN)9] (M = W, Mo) as a building block for the construction of two nona-cyanometalate-bridged heterometallic coordination polymers
Qian, Jun; Yoshikawa, Hirofumi; Humphrey, Mark G.; Zhang, Jinfang; Awaga, Kunio; Zhang, Chi; CrystEngComm 21 (2019) 4363–; doi:10.1039/C9CE00579J

data_7232934
_publ_section_title
;
 In situ formed [M(CN)9] (M = W, Mo) as a building block for the
 construction of two nona-cyanometalate-bridged heterometallic
 coordination polymers
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4363
_journal_paper_doi               10.1039/C9CE00579J
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C33 H16 Mn2 N17 O6 W'
_chemical_formula_weight         1040.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-04-10 deposited with the CCDC.    2019-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.470(2)
_cell_length_b                   14.470(2)
_cell_length_c                   28.017(6)
_cell_measurement_reflns_used    2880
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7858
_cell_measurement_theta_min      2.8154
_cell_volume                     5866.2(17)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            7368
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.003
_diffrn_reflns_theta_min         3.169
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.487
_refine_diff_density_min         -3.213
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2880
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.409
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0742P)^2^+40.3077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2651
_reflns_number_total             2880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00579j2.cif
_cod_data_source_block           s
_cod_depositor_comments
'Adding full bibliography for 7232934--7232935.cif.'
_cod_original_cell_volume        5866(2)
_cod_database_code               7232934
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              19290
_shelx_fab_checksum              6297