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_7048963
_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
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_audit_update_record
;
2019-02-08 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.222(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3915(3)
_cell_length_b                   18.3739(5)
_cell_length_c                   15.2729(5)
_cell_measurement_reflns_used    4323
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      72.1860
_cell_measurement_theta_min      4.8110
_cell_volume                     2543.01(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   30.00   98.00   1.0000    4.3400
omega____ theta____ kappa____ phi______ frames
    -       36.4577   19.0000    0.0000 68

  2 omega   39.00   76.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 37

  3 omega   53.00   78.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 25

  4 omega   41.00  124.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 83

  5 omega  120.00  175.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 55

  6 omega  117.00  169.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 52

  7 omega   92.00  168.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  150.0000 76

  8 omega   73.00  108.00   1.0000    4.3400
omega____ theta____ kappa____ phi______ frames
    -       36.4577  178.0000    0.0000 35

  9 omega   42.00   69.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 27

 10 omega   62.00   88.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 26

 11 omega   44.00  107.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -150.0000 63

 12 omega   54.00   87.00   1.0000    4.3400
omega____ theta____ kappa____ phi______ frames
    -       36.4577 -178.0000 -150.0000 33

 13 omega   39.00  116.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 77

 14 omega   31.00   74.00   1.0000    4.3400
omega____ theta____ kappa____ phi______ frames
    -       36.4577  -99.0000   60.0000 43

 15 omega  -25.00   28.00   1.0000    4.3400
omega____ theta____ kappa____ phi______ frames
    -       36.4577  -38.0000  150.0000 53

 16 omega   22.00   95.00   1.0000    4.3400
omega____ theta____ kappa____ phi______ frames
    -       36.4577   57.0000   30.0000 73

 17 omega   57.00   86.00   1.0000    4.3400
omega____ theta____ kappa____ phi______ frames
    -       36.4577  178.0000 -180.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1134988000
_diffrn_orient_matrix_UB_12      0.0064536000
_diffrn_orient_matrix_UB_13      0.0562757000
_diffrn_orient_matrix_UB_21      0.1071592000
_diffrn_orient_matrix_UB_22      -0.0396041000
_diffrn_orient_matrix_UB_23      0.0796311000
_diffrn_orient_matrix_UB_31      0.0673204000
_diffrn_orient_matrix_UB_32      0.0736270000
_diffrn_orient_matrix_UB_33      0.0377793000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9408
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         4.814
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.404
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38015
_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    2.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.504
_refine_diff_density_min         -5.658
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4490
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+34.8180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3969
_reflns_number_total             4490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00119k2.cif
_cod_data_source_block           160607a
_cod_depositor_comments
'Adding full bibliography for 7048962--7048966.cif.'
_cod_original_cell_volume        2543.00(14)
_cod_database_code               7048963
_chemical_oxdiff_formula         'Co C H O N Mo'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Rigid body (RIGU) restrains
 Mo1, Mo2, O4, O7, C12, N1, C6, C18, C5, C11, C17, N2, C4, N3, C10, N4, C16,
 C1, C3, C7, C9, C13, C15, C2, C8, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              4590
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'