Two novel zipper-like compounds of the usual and bivanadyl capped Keggin clusters connected by propeller-shaped complexes
Yu, Yan; Ma, Huiyuan; Pang, Haijun; Li, Shaobin; Yu, Tingting; Liu, Heng; Zhao, Chunyan; Zhang, Zhuanfang; New Journal of Chemistry 38 (2014) 1271–; doi:10.1039/c3nj01329d

data_7053887
_publ_section_title
;
 Two novel zipper-like compounds of the usual and bivanadyl capped Keggin
 clusters connected by propeller-shaped complexes
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1271
_journal_paper_doi               10.1039/c3nj01329d
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety         'C48 H45 Cu Mo12 N20 O40 P, 4(O)'
_chemical_formula_sum            'C48 H53 Cu Mo12 N20 O44 P'
_chemical_formula_weight         2859.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 100.605(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   22.040(5)
_cell_length_b                   14.850(5)
_cell_length_c                   24.821(5)
_cell_measurement_reflns_used    4915
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.27
_cell_volume                     7985(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22622
_diffrn_reflns_theta_full        24.75
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    2.204
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5488.0
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.150
_refine_diff_density_min         -2.819
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         6778
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+927.4582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2100
_refine_ls_wR_factor_ref         0.2189
_reflns_number_gt                5253
_reflns_number_total             6843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj01329d.txt
_cod_data_source_block           yy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'monoclinic ' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7053887