Assembly of new organic‒inorganic hybrids based on copper-bis(triazole) complexes and Keggin-type polyoxometalates with different negative charges
Hao, Xiu-Li; Ma, Yuan-Yuan; Zhang, Chen; Wang, Qian; Cheng, Xin; Wang, Yong-Hui; Li, Yang-Guang; Wang, En-Bo; CrystEngComm 14 (2012) 6573–; doi:10.1039/c2ce25747e

data_7208750
_publ_section_title
;
 Assembly of new organic--inorganic hybrids based on copper-bis(triazole)
 complexes and Keggin-type polyoxometalates with different negative
 charges
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6573
_journal_paper_doi               10.1039/c2ce25747e
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C36 H43 Cu2 Mo12 N18 O42.5 Si'
_chemical_formula_weight         2714.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.35(3)
_cell_angle_beta                 71.88(3)
_cell_angle_gamma                72.32(3)
_cell_formula_units_Z            1
_cell_length_a                   11.790(2)
_cell_length_b                   12.562(3)
_cell_length_c                   13.051(3)
_cell_measurement_reflns_used    15082
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.08
_cell_volume                     1747.0(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13312
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.796
_exptl_absorpt_correction_T_max  0.5534
_exptl_absorpt_correction_T_min  0.5082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1301
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.001
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       0.00060(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         6118
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1780
_reflns_number_gt                5445
_reflns_number_total             6118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25747e.txt
_cod_data_source_block           h2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1747.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C36 H43 Cu2 Mo12 N18 O42.50 Si'
_cod_database_code               7208750