Ethylene Substitution in a Bis-Ethylene Complex of Rh/Os and Unusual Brønsted−Lowry Basicity of an N-Heterocyclic Carbene
Wells, Kyle D.; Ferguson, Michael J.; McDonald, Robert; Cowie, Martin; Organometallics 30 (2011) 815–; doi:10.1021/om101000y

data_4063872
_publ_section_title
;
 Ethylene Substitution in a Bis-Ethylene Complex of Rh/Os and Unusual
 Br\/onsted&#x2212;Lowry Basicity of an N-Heterocyclic Carbene
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              815
_journal_paper_doi               10.1021/om101000y
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety
'C112 H101 N2 O4 Os2 P8 Rh2, C F3 O3 S, 3.25(C H2 Cl2)'
_chemical_formula_sum            'C116.25 H107.5 Cl6.5 F3 N2 O7 Os2 P8 Rh2 S'
_chemical_formula_weight         2798.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                96.9515(7)
_cell_angle_beta                 106.3856(7)
_cell_angle_gamma                111.1406(6)
_cell_formula_units_Z            2
_cell_length_a                   15.8631(9)
_cell_length_b                   19.6777(11)
_cell_length_c                   21.6108(12)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.26
_cell_volume                     5846.2(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            50247
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    2.779
_exptl_absorpt_correction_T_max  0.6679
_exptl_absorpt_correction_T_min  0.3216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2781
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1381
_refine_ls_number_reflns         25659
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+8.2248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                22035
_reflns_number_total             25659
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om101000y_si_001.cif
_cod_data_source_block           9-trans
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_formula_sum
'C116.25 H107.50 Cl6.50 F3 N2 O7 Os2 P8 Rh2 S'
_cod_database_code               4063872