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_7048966
_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         'C54 H48 Cu3 Mo8 N22 O26, H2 O'
_chemical_formula_sum            'C54 H50 Cu3 Mo8 N22 O27'
_chemical_formula_weight         2397.30
_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   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                109.276(5)
_cell_angle_beta                 105.850(4)
_cell_angle_gamma                104.678(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7419(4)
_cell_length_b                   13.8200(7)
_cell_length_c                   14.4031(7)
_cell_measurement_reflns_used    6651
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8840
_cell_measurement_theta_min      3.2530
_cell_volume                     1797.26(19)
_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
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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)
;
_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  -25.00   23.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5013  -99.0000   60.0000 48

  2 omega  -25.00   23.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5013  -99.0000  -60.0000 48

  3 omega  -14.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7357   19.0000  120.0000 101

  4 omega   -1.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7357   57.0000   30.0000 84

  5 omega  -11.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7357   77.0000  -90.0000 94

  6 omega  -52.00   42.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7357  -77.0000  150.0000 94

  7 omega  -32.00   52.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5013   57.0000    0.0000 84

  8 omega  -25.00    4.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7357  -99.0000  -90.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0337075000
_diffrn_orient_matrix_UB_12      -0.0020732000
_diffrn_orient_matrix_UB_13      0.0357347000
_diffrn_orient_matrix_UB_21      -0.0162857000
_diffrn_orient_matrix_UB_22      0.0460737000
_diffrn_orient_matrix_UB_23      -0.0020785000
_diffrn_orient_matrix_UB_31      -0.0640089000
_diffrn_orient_matrix_UB_32      -0.0363743000
_diffrn_orient_matrix_UB_33      -0.0439411000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22203
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.638
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97278
_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    2.215
_exptl_crystal_F_000             1167
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0299P)^2^+0.7217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5464
_reflns_number_total             7347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00119k2.cif
_cod_data_source_block           160403a
_cod_depositor_comments
'Adding full bibliography for 7048962--7048966.cif.'
_cod_original_cell_volume        1797.27(15)
_cod_database_code               7048966
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu C H O N Mo'
_reflns_odcompleteness_completeness 99.92
_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
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 O1W
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
3. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C18(H18A,H18B), C6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C21(H21), C22(H22), C25(H25), C24(H24), C4(H4), C13(H13), C1(H1),
 C3(H3), C2(H2), C14(H14), C16(H16), C10(H10), C15(H15), C7(H7), C9(H9), C8(H8)
;
_shelx_res_checksum              61730
_olex2_submission_special_instructions 'No special instructions were received'