Assembling [M(P4Mo6)2] (M = Na, Mn, Na/Cu) dimeric clusters via transition metal/sodium ions into 0D to 3D phosphomolybdates
Li, Wei; Zhu, Jian-Nan; Shen, Nan-Nan; Xiong, Wei-Wei; Huang, Xiao-Ying; CrystEngComm 21 (2019) 971–; doi:10.1039/C8CE01866A

data_7232171
_publ_section_title
;
 Assembling [M(P4Mo6)2] (M = Na, Mn, Na/Cu) dimeric clusters via
 transition metal/sodium ions into 0D to 3D phosphomolybdates
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              971
_journal_paper_doi               10.1039/C8CE01866A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C20 H68 Mn2.5 Mo12 N8 Na2 O71.5 P8'
_chemical_formula_weight         3147.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-10-30 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.869(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6598(4)
_cell_length_b                   13.3538(4)
_cell_length_c                   22.0021(6)
_cell_measurement_reflns_used    9017
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8250
_cell_measurement_theta_min      3.5570
_cell_volume                     4181.6(2)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  Xcalibur
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25587
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.315
_diffrn_reflns_theta_min         3.370
_exptl_absorpt_coefficient_mu    2.383
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_description       flake
_exptl_crystal_F_000             3049
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   0.931
_exptl_transmission_factor_min   0.570
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1292
_refine_ls_number_reflns         15155
_refine_ls_number_restraints     1411
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+24.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                13417
_reflns_number_total             15155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01866a2.cif
_cod_data_source_block           x_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7232169--7232174.cif.'
_cod_original_formula_sum        'C20 H68 Mn2.50 Mo12 N8 Na2 O71.50 P8'
_cod_database_code               7232171
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              1072