Bis[<i>trans</i>-difluoridotetrakis(pyridine-κ<i>N</i>)chromium(III)] sodium tetrachloridozincate perchlorate from synchrotron data
Moon, Dohyun; Ryoo, Keon Sang; Choi, Jong-Ha; Acta Crystallographica Section E 70 (2014) m280–; doi:10.1107/S1600536814014408

data_2239670
_publ_section_title
;
 Bis[<i>trans</i>-difluoridotetrakis(pyridine-\k<i>N</i>)chromium(III)]
 sodium tetrachloridozincate perchlorate from synchrotron data
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m280
_journal_paper_doi               10.1107/S1600536814014408
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Na [Cr F2 (C5 H5 N)4]2 [Zn Cl4] Cl O4'
_chemical_formula_moiety
'2(C20 H20 Cr F2 N4 +), Na +, Cl O4 -, Cl4 Zn 2-'
_chemical_formula_sum            'C40 H40 Cl5 Cr2 F4 N8 Na O4 Zn'
_chemical_formula_weight         1142.41
_chemical_name_systematic
;
Bis[<i>trans</i>-difluoridotetrakis(pyridine-\k<i>N</i>)chromium(III)]
sodium tetrachloridozincate perchlorate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.397(5)
_cell_length_b                   14.600(3)
_cell_length_c                   25.510(5)
_cell_measurement_reflns_used    237022
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.547
_cell_measurement_theta_min      0.361
_cell_volume                     9459(3)
_computing_cell_refinement       '<i>HKL3000sm</i> (Otwinowski & Minor, 1997)'
_computing_data_collection
;
<i>PAL ADSC Quantum-210 ADX</i> (Arvai & Nielsen, 1983)
;
_computing_data_reduction        '<i>HKL3000sm</i> (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  '<i>XL</i> in SHELXL2014 (Sheldrick, 2008)'
_computing_structure_solution    '<i>XS</i> in SHELXS2014 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.62998
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            86381
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.009
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'(<i>HKL3000sm</i>; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             4624
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.989
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         13152
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0773P)^2^+19.7848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                12355
_reflns_number_total             13152
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5321sup1.cf
_cod_data_source_block           I
_cod_database_code               2239670
_cod_database_fobs_code          2239670
_shelx_hkl_checksum              79133
_shelx_res_checksum              40171
_shelxl_version_number           2.014