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_7048964
_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
'4(Mo8 O26), 8(C18 H20 Cu N4 O), 10.67(H2 O), 4(H3 O0.75)'
_chemical_formula_sum            'C144 H193.33 Cu8 Mo32 N32 O125.67'
_chemical_formula_weight         7961.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-08 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.402(5)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   27.2598(9)
_cell_length_b                   11.72354(18)
_cell_length_c                   21.7423(7)
_cell_measurement_reflns_used    4669
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.2570
_cell_measurement_theta_min      3.7940
_cell_volume                     5663.7(4)
_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      293(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  -26.00   33.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -38.0000  -60.0000 59

  2 omega   70.00   96.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327    0.0000  -30.0000 26

  3 omega   47.00   74.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -99.0000   90.0000 27

  4 omega    2.00   29.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -99.0000   90.0000 27

  5 omega   -4.00   55.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327    0.0000  -30.0000 59

  6 omega   91.00  174.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -150.0000 83

  7 omega   73.00  109.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327  178.0000   30.0000 36

  8 omega   41.00  146.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000   30.0000 105

  9 omega   84.00  109.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -90.0000 25

 10 omega   72.00  104.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 32

 11 omega   64.00  115.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 51

 12 omega   57.00   91.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 34

 13 omega   47.00   72.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 25

 14 omega   41.00   87.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 46

 15 omega   42.00   89.00   1.0000   12.8450
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 47

 16 omega   53.00   78.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327 -178.0000 -120.0000 25

 17 omega   55.00   84.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327 -178.0000  -90.0000 29

 18 omega  -27.00   53.00   1.0000    3.2100
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -57.0000 -180.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0154417000
_diffrn_orient_matrix_UB_12      0.0441429000
_diffrn_orient_matrix_UB_13      -0.0536229000
_diffrn_orient_matrix_UB_21      -0.0632618000
_diffrn_orient_matrix_UB_22      -0.0340987000
_diffrn_orient_matrix_UB_23      -0.0684500000
_diffrn_orient_matrix_UB_31      -0.0238687000
_diffrn_orient_matrix_UB_32      0.1189287000
_diffrn_orient_matrix_UB_33      0.0002840000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9845
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.547
_diffrn_reflns_theta_max         66.547
_diffrn_reflns_theta_min         3.979
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.675
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18559
_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            blue
_exptl_crystal_density_diffrn    2.334
_exptl_crystal_F_000             3863
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4362
_reflns_number_total             5000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00119k2.cif
_cod_data_source_block           161012a
_cod_depositor_comments
'Adding full bibliography for 7048962--7048966.cif.'
_cod_database_code               7048964
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu C H O N Mo'
_reflns_odcompleteness_completeness 99.91
_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. Others
 Fixed Sof: O3W(0.375) H3WA(0.75) H3WB(0.75) O4W(0.33333) H4WA(0.33333)
 H4WB(0.33333)
3.a Riding coordinates:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
3.b Rotating group:
 O1W(H1WA,H1WB)
3.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C18(H18A,H18B), C12(H12A,H12B)
3.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C10(H10), C14(H14), C7(H7), C8(H8), C4(H4), C13(H13),
 C2(H2), C9(H9), C1(H1), C3(H3)
;
_shelx_res_checksum              15486
_olex2_date_sample_data_collection 2016-10-12
_olex2_submission_special_instructions 'No special instructions were received'