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_7048962
_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 Mo N4 O3, 4(H2 O)'
_chemical_formula_sum            'C18 H26 Mo N4 O7'
_chemical_formula_weight         506.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-01-27
_audit_creation_method
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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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4558(2)
_cell_length_b                   13.84247(15)
_cell_length_c                   18.8277(3)
_cell_measurement_reflns_used    4179
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      71.7640
_cell_measurement_theta_min      4.7070
_cell_volume                     4288.74(10)
_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    '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 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   59.00  102.00   1.0000    3.7150
omega____ theta____ kappa____ phi______ frames
    -       36.5827   57.0000    0.0000 43

  2 omega   39.00   65.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 26

  3 omega   57.00   97.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 40

  4 omega   53.00   79.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 26

  5 omega   39.00  110.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   60.0000 71

  6 omega   50.00   76.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 26

  7 omega   40.00   97.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 57

  8 omega   39.00   84.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 45

  9 omega   19.00   59.00   1.0000    3.7150
omega____ theta____ kappa____ phi______ frames
    -       36.5827   38.0000  150.0000 40

 10 omega   25.00  103.00   1.0000    3.7150
omega____ theta____ kappa____ phi______ frames
    -       36.5827   77.0000 -120.0000 78

 11 omega   57.00  109.00   1.0000    3.7150
omega____ theta____ kappa____ phi______ frames
    -       36.5827  178.0000 -150.0000 52

 12 omega   26.00   66.00   1.0000    3.7150
omega____ theta____ kappa____ phi______ frames
    -       36.5827   57.0000 -150.0000 40

 13 omega   41.00   88.00   1.0000   14.8500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0188777000
_diffrn_orient_matrix_UB_12      -0.0312834000
_diffrn_orient_matrix_UB_13      -0.0767889000
_diffrn_orient_matrix_UB_21      -0.0880332000
_diffrn_orient_matrix_UB_22      0.0236386000
_diffrn_orient_matrix_UB_23      -0.0217455000
_diffrn_orient_matrix_UB_31      0.0256061000
_diffrn_orient_matrix_UB_32      0.1041545000
_diffrn_orient_matrix_UB_33      -0.0181081000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.211
_diffrn_reflns_theta_min         4.697
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45457
_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            colorless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0512P)^2^+1.2427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3546
_reflns_number_total             4166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00119k2.cif
_cod_data_source_block           160731a
_cod_depositor_comments
'Adding full bibliography for 7048962--7048966.cif.'
_cod_database_code               7048962
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O3W(H3WA,H3WB), O1W(H1WA,H1WB), O4W(H4WA,H4WB), O2W(H2WA,H2WB)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C7(H7), C10(H10), C13(H13), C4(H4), C1(H1), C15(H15), C8(H8),
 C14(H14), C9(H9), C2(H2), C3(H3)
;
_shelx_res_checksum              95256
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-31
_olex2_submission_special_instructions 'No special instructions were received'