X-ray Absorption Spectroscopic Studies of Chromium Nitroso Complexes. Crystal and Molecular Structure of (Ph4P)3[Cr(NO)(NCS)5].2.4(CH3)2CO
Aviva Levina; Peter Turner; Peter A. Lay; Inorganic Chemistry 42 (2003) 5392–5398; doi:10.1021/ic0340480

data_4314023
_publ_contact_author_address
;    
  The Centre for Heavy Metal Research, 
  School of Chemistry, 
  University of Sydney, 
  Sydney 2006, NSW, Australia. 
;
_publ_contact_author_email       p.lay@chem.usyd.edu.au
_publ_contact_author_fax         '+61 2 9351 3329'
_publ_contact_author_name        'Peter A. Lay'
_publ_contact_author_phone       '+61 2 9351 4269'
_publ_section_title
;
 X-ray Absorption Spectroscopic Studies of Chromium Nitroso Complexes.
 Crystal and Molecular Structure of (Ph4P)3[Cr(NO)(NCS)5].2.4(CH3)2CO
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5392
_journal_page_last               5398
_journal_paper_doi               10.1021/ic0340480
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C84.2 H74.4 Cr N6 O3.4 P3 S5'
_chemical_formula_weight         1529.91
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.902(7)
_cell_angle_beta                 78.326(7)
_cell_angle_gamma                71.572(7)
_cell_formula_units_Z            2
_cell_length_a                   13.401(6)
_cell_length_b                   17.707(7)
_cell_length_c                   18.773(8)
_cell_measurement_reflns_used    1008
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.245
_cell_measurement_theta_min      2.525
_cell_volume                     4088(3)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics
;
  teXsan for Windows (MSC, 1997) 
  xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999)
  ORTEPII  (Johnson,C.K., 1976). 
  WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41171
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0.09
_diffrn_standards_number         171
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
  Gaussian (Coppens et al., 1965) 
  XPREP  (Bruker, 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.357
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         19242
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.384
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^+0.8P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                12196
_reflns_number_total             19242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0340480si20030116_100857.cif
_cod_data_source_block           pal55
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C84.20 H74.40 Cr N6 O3.40 P3 S5'
_cod_database_code               4314023