Synthesis and characterization of a series of novel polyoxometalate-supported carbonyl manganese derivatives
Jia, Jiage; Zhang, Yanhui; Zhang, Panpan; Ma, Pengtao; Zhang, Dongdi; Wang, Jingping; Niu, Jingyang; RSC Adv.  (2016) –; doi:10.1039/C6RA23547F

data_7227018
_publ_section_title
;
 Synthesis and characterization of a series of novel
 polyoxometalate-supported carbonyl manganese derivatives
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA23547F
_journal_year                    2016
_chemical_formula_moiety
'0.5(C12 Mn12 Na12 O210 Sb4 W36), 2(C4 H12 N), 13(O)'
_chemical_formula_sum            'C14 H116 Mn6 N2 Na6 O118 Sb2 W18'
_chemical_formula_weight         6221.46
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-21 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.4654(12)
_cell_length_b                   14.4945(10)
_cell_length_c                   25.9004(18)
_cell_measurement_reflns_used    7391
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.20
_cell_volume                     5959.9(7)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29605
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.902
_exptl_absorpt_coefficient_mu    18.489
_exptl_absorpt_correction_T_max  0.1061
_exptl_absorpt_correction_T_min  0.0641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         10572
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0264P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8227
_reflns_number_total             10572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra23547f2.cif
_cod_data_source_block           njy1
_cod_database_code               7227018
_shelx_estimated_absorpt_t_max   0.106
_shelx_estimated_absorpt_t_min   0.064
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C4
 1.47 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim C4 \\sim C7: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O6W)
\\sim Ueq, Uanis(O21W) \\sim Ueq, Uanis(O22W) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O23W(0.5) O24W(0.5)
5.a Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'