Low-temperature redetermination of hexakis(μ-chloroacetato-κ^2^<i>O</i>:<i>O</i>')-μ~3~-oxido-tris[aquachromium(III)] nitrate 3.5-hydrate
Ng, Seik Weng; Acta Crystallographica Section E 64 (2008) m1102–; doi:10.1107/S1600536808023805

data_2219060
_publ_section_title
;Low-temperature redetermination of
 hexakis(\m-chloroacetato-\k^2^<i>O</i>:<i>O</i>')-\m~3~-oxido-tris[aquachromium(III)]
 nitrate 3.5-hydrate
;
_journal_coeditor_code           HY2147
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1102
_journal_paper_doi               10.1107/S1600536808023805
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Cr3 (C2 H2 Cl O2)6 O (H2 O)3] N O3, 3.5H2 O'
_chemical_formula_moiety         'C12 H18 Cl6 Cr3 O16 +, N O3 -, 3.5(H2 O)'
_chemical_formula_sum            'C12 H25 Cl6 Cr3 N O22.5'
_chemical_formula_weight         912.03
_chemical_name_systematic
;
hexakis(\m-chloroacetato-\k^2^<i>O</i>:<i>O</i>')-\m~3~-oxido-
tris[aquachromium(III)] nitrate 3.5-hydrate
;
_space_group_IT_number           14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.2930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4938(2)
_cell_length_b                   14.7622(2)
_cell_length_c                   17.2687(3)
_cell_measurement_reflns_used    7530
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.4
_cell_volume                     3165.78(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39914
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular chip'
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7271
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+3.1321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                5349
_reflns_number_total             7271
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2147.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2219060
_cod_database_fobs_code          2219060