Isopolymolybdate-based inorganic-organic hybrid compounds constructed by multidentate N-donor ligands: syntheses, structures and properties.
Guo, Haiyang; Gong, Chunhua; Zeng, Xianghua; Xu, Hao; Zeng, Qingdao; Zhang, Junyong; Xie, Jingli; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5541–5550; doi:10.1039/c9dt00119k

data_7048965
_publ_section_title
;
 Isopolymolybdate-based inorganic-organic hybrid compounds constructed by
 multidentate N-donor ligands: syntheses, structures and properties.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5541
_journal_page_last               5550
_journal_paper_doi               10.1039/c9dt00119k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C18 H18 Co Mo4 N4 O13'
_chemical_formula_sum            'C18 H18 Co Mo4 N4 O13'
_chemical_formula_weight         941.05
_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
_audit_creation_date             2019-01-27
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Olex2 1.2-alpha
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_audit_update_record
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2019-02-08 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.806(3)
_cell_angle_gamma                90
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_cell_length_a                   9.8656(3)
_cell_length_b                   19.4521(4)
_cell_length_c                   13.8036(3)
_cell_measurement_reflns_used    4327
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.0270
_cell_measurement_theta_min      3.1740
_cell_volume                     2535.86(12)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
  1 omega   22.00   51.75   0.8500    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2084   77.0000  120.0000 35

  2 omega   -9.00   88.75   0.8500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4428   77.0000   30.0000 115

  3 omega  -42.00   47.25   0.8500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4428  -77.0000  -90.0000 105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0099094000
_diffrn_orient_matrix_UB_12      0.0343562000
_diffrn_orient_matrix_UB_13      0.0179280000
_diffrn_orient_matrix_UB_21      0.0249587000
_diffrn_orient_matrix_UB_22      -0.0122508000
_diffrn_orient_matrix_UB_23      0.0504400000
_diffrn_orient_matrix_UB_31      0.0701067000
_diffrn_orient_matrix_UB_32      -0.0004899000
_diffrn_orient_matrix_UB_33      -0.0038920000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11183
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.298
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.665
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5204
_reflns_number_total             5849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00119k2.cif
_cod_data_source_block           160123a
_cod_depositor_comments
'Adding full bibliography for 7048962--7048966.cif.'
_cod_original_cell_volume        2535.86(10)
_cod_database_code               7048965
_chemical_oxdiff_formula         'Co1 C18 N4 H18 N2 Mo7 O24'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C6(H6A,H6B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C16(H16), C3(H3), C4(H4), C2(H2), C13(H13), C15(H15), C7(H7),
 C14(H14), C10(H10), C9(H9), C8(H8)
;
_shelx_res_checksum              22817
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'