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_7232172
_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_absolute_configuration unk
_chemical_formula_sum            'C3 H58 Mn2.5 Mo12 N5.5 Na4.5 O72.5 P8'
_chemical_formula_weight         2971.39
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 2 2'
_symmetry_space_group_name_Hall  'P 4cw 2c'
_symmetry_space_group_name_H-M   'P 43 2 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.39830(10)
_cell_length_b                   13.39830(10)
_cell_length_c                   38.3301(8)
_cell_measurement_reflns_used    9349
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.1430
_cell_measurement_theta_min      3.8410
_cell_volume                     6880.81(16)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  xcalibur
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            18174
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.230
_diffrn_reflns_theta_min         3.400
_exptl_absorpt_coefficient_mu    2.900
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82509
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.868
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             5722
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.647
_exptl_transmission_factor_min   0.534
_refine_diff_density_max         1.217
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7634
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0450P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                7351
_reflns_number_total             7634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01866a2.cif
_cod_data_source_block           x_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7232169--7232174.cif.'
_cod_original_cell_volume        6880.81(18)
_cod_original_formula_sum        'C3 H58 Mn2.50 Mo12 N5.50 Na4.50 O72.50 P8'
_cod_database_code               7232172
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              89951