Crystal structure of <i>trans</i>-difluoridotetrakis(pyridine-κ<i>N</i>)chromium(III) trichlorido(pyridine-κ<i>N</i>)zincate monohydrate from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 70 (2014) 290–293; doi:10.1107/S160053681402145X

data_2240028
_publ_section_title
;
 Crystal structure of
 <i>trans</i>-difluoridotetrakis(pyridine-\k<i>N</i>)chromium(III)
 trichlorido(pyridine-\k<i>N</i>)zincate monohydrate from synchrotron data
;
_journal_coeditor_code           LH5726
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              290
_journal_page_last               293
_journal_paper_doi               10.1107/S160053681402145X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Cr F2 (C5 H5 N)4] [Zn Cl3 (C5 H5 N)], H2 O'
_chemical_formula_moiety         'C20 H20 Cr F2 N4 +, C5 H5 Cl3 N Zn -, H2 O'
_chemical_formula_sum            'C25 H27 Cl3 Cr F2 N5 O Zn'
_chemical_formula_weight         675.23
_chemical_name_systematic
;
<i>trans</i>-Difluoridotetrakis-(pyridine-\k<i>N</i>)chromium(III)
trichlorido(pyridine-\k<i>N</i>)zincate monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                103.69(3)
_cell_angle_beta                 105.07(3)
_cell_angle_gamma                101.25(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1350(18)
_cell_length_b                   12.852(3)
_cell_length_c                   13.607(3)
_cell_measurement_reflns_used    70974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.547
_cell_measurement_theta_min      0.361
_cell_volume                     1441.6(7)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL ADSC Quantum-210 ADX Software</i> (Arvai & Nielsen, 1983)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2007),
Mercury (Macrae <i>et al.</i>, 2006) and
PLATON (Spek, 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.62998
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15474
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.128
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm</i> Scalepack; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       rod
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.849
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7929
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+1.3104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                7758
_reflns_number_total             7929
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5726sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1441.6(6)
_cod_database_code               2240028
_cod_database_fobs_code          2240028
_shelx_hkl_checksum              48855
_shelx_res_checksum              43382
_shelxl_version_number           2014/6