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_7232935
_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            'C45 H44 Mn2 Mo N21 O10'
_chemical_formula_weight         1244.83
_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_block_doi                 10.5517/cczth4d
_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                   14.450(2)
_cell_length_b                   14.450(2)
_cell_length_c                   28.044(6)
_cell_measurement_reflns_used    3030
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.363
_cell_measurement_theta_min      3.172
_cell_volume                     5855.7(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 0.994
_diffrn_measured_fraction_theta_max 0.985
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11222
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         3.172
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2595
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3030
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1134P)^2^+15.4149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2841
_reflns_number_total             3030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00579j2.cif
_cod_data_source_block           a_sq_s
_cod_depositor_comments
'Adding full bibliography for 7232934--7232935.cif.'
_cod_original_cell_volume        5856(2)
_cod_database_code               7232935
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              15245
_shelx_fab_checksum              81233