Construction of 3D metal‒organic frameworks bearing heteropolyoxometalate units and multi-azole molecules and exploration of their photocatalytic activities
Gong, Chunhua; Zeng, Xianghua; Xin, Li; Zhang, Junyong; Xie, Jingli; RSC Adv. 7 (2017) 36860–; doi:10.1039/C7RA05210C

data_7228751
_publ_section_title
;
 Construction of 3D metal--organic frameworks bearing
 heteropolyoxometalate units and multi-azole molecules and exploration of
 their photocatalytic activities
;
_journal_issue                   59
_journal_name_full               'RSC Adv.'
_journal_page_first              36860
_journal_paper_doi               10.1039/C7RA05210C
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C36 H30 Cr Cu5 Mo6 N28 O31'
_chemical_formula_sum            'C36 H30 Cr Cu5 Mo6 N28 O31'
_chemical_formula_weight         2296.22
_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     iterative
_audit_creation_date             2016-04-06
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;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-03 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                107.916(4)
_cell_angle_beta                 103.921(3)
_cell_angle_gamma                112.783(4)
_cell_formula_units_Z            1
_cell_length_a                   12.8771(6)
_cell_length_b                   13.4775(6)
_cell_length_c                   13.5993(5)
_cell_measurement_reflns_used    6947
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.3360
_cell_measurement_theta_min      3.0450
_cell_volume                     1888.45(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
;
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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.998
_diffrn_measurement_details
;
  1 omega   15.00   80.45   0.8500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8919   77.0000  -60.0000 77

  2 omega    8.00   44.55   0.8500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5013   77.0000 -150.0000 43

  3 omega   16.00   82.30   0.8500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8919   77.0000   90.0000 78

  4 omega   -8.00   64.25   0.8500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8919   77.0000   30.0000 85

  5 omega  -11.00   35.75   0.8500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8919   77.0000  -90.0000 55

  6 omega  -41.00   51.65   0.8500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5013   77.0000  150.0000 109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0353385000
_diffrn_orient_matrix_UB_12      -0.0082453000
_diffrn_orient_matrix_UB_13      -0.0536600000
_diffrn_orient_matrix_UB_21      -0.0530591000
_diffrn_orient_matrix_UB_22      -0.0461603000
_diffrn_orient_matrix_UB_23      -0.0023319000
_diffrn_orient_matrix_UB_31      -0.0150511000
_diffrn_orient_matrix_UB_32      0.0433255000
_diffrn_orient_matrix_UB_33      0.0269654000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13711
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.798
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84078
_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    2.019
_exptl_crystal_F_000             1111
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         2.825
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0393P)^2^+4.8027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5836
_reflns_number_total             6634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra05210c2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1888.46(15)
_cod_database_code               7228751
_chemical_oxdiff_formula         'Cu1 C9 N7 H9 Cr1 Mo6 O23'
_exptl_absorpt_special_details   block
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5)
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              91122
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'