[(ZnSb6)2]4-: a new structure type for coupled norbornadiene-like subunits
Wang, Yi; Zavalij, Peter Y.; Eichhorn, Bryan W.; Chem. Commun.  (2017) –; doi:10.1039/C7CC07454A

data_7120735
_publ_section_title
;
 [(ZnSb6)2]4-: a new structure type for coupled norbornadiene-like
 subunits
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC07454A
_journal_year                    2017
_chemical_formula_moiety         '4(C18 H36 K N2 O6), Sb12 Zn2, 0.65(C7 H8)'
_chemical_formula_sum            'C76.55 H146.2 K4 N8 O24 Sb12 Zn2'
_chemical_formula_weight         3310.95
_chemical_name_systematic        'Sb12Zn4 cluster'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014 & ZCIF'
_audit_update_record
;
2017-08-08 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.3679(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.346(3)
_cell_length_b                   14.3599(11)
_cell_length_c                   26.819(2)
_cell_measurement_reflns_used    14786
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.3
_cell_measurement_theta_min      2.2
_cell_volume                     11822.4(17)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'Olex2 (Dolomanov, 2009), Crystal Maker'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0237572
_diffrn_orient_matrix_UB_12      -0.0549578
_diffrn_orient_matrix_UB_13      -0.0028827
_diffrn_orient_matrix_UB_21      0.0137009
_diffrn_orient_matrix_UB_22      -0.0098346
_diffrn_orient_matrix_UB_23      0.0322254
_diffrn_orient_matrix_UB_31      -0.0281317
_diffrn_orient_matrix_UB_32      0.0416213
_diffrn_orient_matrix_UB_33      0.0037932
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            104237
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.851
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.291
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6406
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.881
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1611
_refine_ls_number_reflns         20801
_refine_ls_number_restraints     4609
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+147.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13210
_reflns_number_total             20801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07454a2.cif
_cod_data_source_block           2819
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        11822.3(16)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C76.55 H146.20 K4 N8 O24 Sb12 Zn2'
_cod_database_code               7120735
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.384
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              11706