An unusual mono-substituted Keggin anion-chain based 3D framework with 24-membered macrocycles as linker units
Pang, Haijun; Ma, Huiyuan; Yu, Yan; Yang, Ming; Xun, Ye; Liu, Bo; Journal of Solid State Chemistry 186 (2012) 23–28; doi:10.1016/j.jssc.2011.11.032

data_1563034
_publ_section_title
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 An unusual mono-substituted Keggin anion-chain based 3D framework with
 24-membered macrocycles as linker units
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_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              23
_journal_page_last               28
_journal_paper_doi               10.1016/j.jssc.2011.11.032
_journal_volume                  186
_journal_year                    2012
_chemical_formula_sum            'C52 H60 Cu4 N8 O40 P W11'
_chemical_formula_weight         3744.59
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_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                 108.245(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   25.993(7)
_cell_length_b                   14.628(4)
_cell_length_c                   21.521(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     7771(3)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       '\w scan'
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.1293
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19868
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    17.387
_exptl_absorpt_correction_T_max  0.162
_exptl_absorpt_correction_T_min  0.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6756.0
_exptl_crystal_size_max          0.1126
_exptl_crystal_size_mid          0.1117
_exptl_crystal_size_min          0.1109
_refine_diff_density_max         2.227
_refine_diff_density_min         -3.269
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         10597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                5159
_reflns_number_total             10597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2012-186-23.cif
_cod_data_source_block           pp
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        7772(3)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               1563034