[Ni(phen)~3~]~2~Sb~18~S~29~: A Novel Three-Dimensional Framework Thioantimonate(III) Templated by [Ni(phen)~3~] Complexes
Ke-Zhao Du; Mei-Ling Feng; Long-Hua Li; Bing Hu; Zu-Ju Ma; Peng Wang; Jian-Rong Li; Yu-Long Wang; Guo-Dong Zou; Xiao-Ying Huang; Inorganic Chemistry 51 (2012) 3926–3928; doi:10.1021/ic202246q

data_4328761
_publ_contact_author_address
;
State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
_publ_contact_author_email       xyhuang@fjirsm.ac.cn
_publ_contact_author_fax         86-59183793727
_publ_contact_author_name        'Prof Xiao-Ying Huang'
_publ_contact_author_phone       86-59183793727
_publ_section_title
;
 [Ni(phen)~3~]~2~Sb~18~S~29~: A Novel Three-Dimensional Framework
 Thioantimonate(III) Templated by [Ni(phen)~3~] Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3926
_journal_page_last               3928
_journal_paper_doi               10.1021/ic202246q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'S29 Sb18, 2(C36 H24 N6 Ni)'
_chemical_formula_sum            'C72 H48 N12 Ni2 S29 Sb18'
_chemical_formula_weight         4319.88
_chemical_name_systematic
; 
 ? 
;
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_cell_angle_alpha                90.00
_cell_angle_beta                 106.5568(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.17374(16)
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_cell_length_c                   12.37007(19)
_cell_measurement_reflns_used    12916
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5427
_cell_measurement_theta_min      2.3780
_cell_volume                     5471.76(14)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
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_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2083
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
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_diffrn_reflns_theta_full        26.05
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.622
_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), 5671 Friedel pairs'
_refine_ls_abs_structure_Flack   0.066(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         17271
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0380P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                16490
_reflns_number_total             17271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202246q_si_002.cif
_cod_data_source_block           compound-1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4328761