Chalcogen extrusion from heteroallenes and carbon monoxide by a three-coordinate rh(i) disilylamide.
Whited, Matthew T.; Qiu, Lisa; Kosanovich, Alex J.; Janzen, Daron E.; Inorganic chemistry 54 (2015) 3670–3679; doi:10.1021/acs.inorgchem.5b00305

data_4346106
_publ_section_title
;
 Chalcogen extrusion from heteroallenes and carbon monoxide by a
 three-coordinate rh(i) disilylamide.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3670
_journal_page_last               3679
_journal_paper_doi               10.1021/acs.inorgchem.5b00305
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C37 H80 P4 Rh2 S3, C4 H10 O'
_chemical_formula_sum            'C41 H90 O P4 Rh2 S3'
_chemical_formula_weight         1025.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.349(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2078(19)
_cell_length_b                   20.257(3)
_cell_length_c                   22.118(4)
_cell_measurement_reflns_used    2964
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      20.58
_cell_measurement_theta_min      2.21
_cell_volume                     4999.7(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.1037
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50650
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         1.825
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.9697
_exptl_absorpt_correction_T_min  0.8652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0734 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.8922.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.609
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         11463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7183
_reflns_number_total             11463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00305_si_002.cif
_cod_data_source_block           UMN15007_compound3
_cod_original_cell_volume        4999.9(15)
_cod_database_code               4346106
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.872
_shelx_res_checksum              8760
_shelx_hkl_checksum              56783