A molecular corner: <i>fac</i>-tricarbonylchloridobis[3-(4-pyridyl)pentane-2,4-dione-κ<i>N</i>]rhenium(I) chloroform solvate
Kakoullis Jr, James; Maverick, Andrew W.; Fronczek, Frank R.; Acta Crystallographica Section E 63 (2007) m1360–m1361; doi:10.1107/S1600536807016996

data_2213590
_publ_section_title
;A molecular corner:
 <i>fac</i>-tricarbonylchloridobis[3-(4-pyridyl)pentane-2,4-dione-\k<i>N</i>]rhenium(I)
 chloroform solvate
;
_journal_coeditor_code           TK2147
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1360
_journal_page_last               m1361
_journal_paper_doi               10.1107/S1600536807016996
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Re Cl (C10 H11 N O2)2 (C O)3], C H Cl3'
_chemical_formula_moiety         'C23 H22 Cl N2 O7 Re, C H Cl3'
_chemical_formula_sum            'C24 H23 Cl4 N2 O7 Re'
_chemical_formula_weight         779.44
_chemical_name_systematic
;fac-tricarbonylchloridobis[3-(4-pyridyl)pentane-2,4-dione-\k<i>N</i>]rhenium(I)
chloroform
 solvate
;
_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
_cell_angle_beta                 102.477(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.889(4)
_cell_length_b                   11.607(4)
_cell_length_c                   24.306(10)
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    110
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.5
_cell_volume                     2999(2)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'SCALEPACK and DENZO  (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'Nonius KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_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  0.071
_diffrn_reflns_av_sigmaI/netI    0.065
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27300
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.450
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.97
_refine_diff_density_min         -1.80
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.373
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.373
_refine_ls_R_factor_all          0.093
_refine_ls_R_factor_gt           0.058
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+2.57P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.137
_refine_ls_wR_factor_ref         0.151
_reflns_number_gt                4148
_reflns_number_total             5749
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2147.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_cell_volume        3000(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2213590
_cod_database_fobs_code          2213590