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_7227020
_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
'Bi2 C6 Mn5.5 O82 W18.5, 2(Mn O6), 2(C4 H12 N), 12(O)'
_chemical_formula_sum            'C14 H92 Bi2 Mn7.5 N2 O106 W18.5'
_chemical_formula_weight         6216.13
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                76.453(4)
_cell_angle_beta                 85.953(4)
_cell_angle_gamma                63.542(4)
_cell_formula_units_Z            1
_cell_length_a                   12.663(3)
_cell_length_b                   13.412(3)
_cell_length_c                   20.342(5)
_cell_measurement_reflns_used    1714
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.53
_cell_volume                     3004.6(12)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.1375
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15353
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         1.811
_exptl_absorpt_coefficient_mu    21.400
_exptl_absorpt_correction_T_max  0.1536
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1300 before and 0.0419 after correction.
The Ratio of minimum to maximum transmission is 0.3965.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.378
_refine_diff_density_min         -2.851
_refine_diff_density_rms         0.418
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         10592
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0510P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6373
_reflns_number_total             10592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra23547f2.cif
_cod_data_source_block           njy1
_cod_original_cell_volume        3004.9(13)
_cod_original_formula_sum        'C14 H92 Bi2 Mn7.50 N2 O106 W18.50'
_cod_database_code               7227020
_shelx_estimated_absorpt_t_max   0.154
_shelx_estimated_absorpt_t_min   0.094
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C4 = N1-C5 = N1-C6 = N1-C7
 1.47 with sigma of 0.01
 C4-C5 \\sim C4-C6 \\sim C4-C7 \\sim C5-C6 \\sim C5-C7 \\sim C6-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(C2)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: W10(0.25) Mn1(0.75)
 Fixed Uiso: O16W(0.11258) O17W(0.14744)
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'