Hexa-μ~2~-acetato-κ^12^<i>O</i>:<i>O</i>'-(azido-κ<i>N</i>)bis(methanol-κ<i>O</i>)-μ~3~-oxido-trichromium(III) methanol monosolvate
Jiang, Guo-Qing; Li, Jian-Hua; Wang, Miao; Shi, Yu-Jun; Acta Crystallographica Section E 67 (2011) m1483–; doi:10.1107/S1600536811039699

data_2232215
_publ_section_title
;
 Hexa-\m~2~-acetato-\k^12^<i>O</i>:<i>O</i>'-(azido-\k<i>N</i>)bis(methanol-\k<i>O</i>)-\m~3~-oxido-trichromium(III)
 methanol monosolvate
;
_journal_coeditor_code           DS2137
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1483
_journal_paper_doi               10.1107/S1600536811039699
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cr3 (C2 H3 O2)6 (N3) O (C H4 O)2], C H4 O'
_chemical_formula_moiety         'C14 H26 Cr3 N3 O15, C H4 O'
_chemical_formula_sum            'C15 H30 Cr3 N3 O16'
_chemical_formula_weight         664.42
_chemical_name_systematic
;
Hexa-\m~2~-acetato-\k^12^<i>O</i>:<i>O</i>'-(azido-\k<i>N</i>)bis(methanol-
\k<i>O</i>)-\m~3~-oxido-trichromium(III) methanol monosolvate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 130.484(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.165(5)
_cell_length_b                   10.609(3)
_cell_length_c                   15.641(4)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.3
_cell_volume                     2671.2(12)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6800
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.474
_refine_ls_abs_structure_details 'Flack (1983), <b>1110 Friedel pairs</b>'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3692
_refine_ls_number_restraints     986
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+7.9006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                3155
_reflns_number_total             3692
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ds2137.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2232215
_cod_database_fobs_code          2232215