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_4346108
_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         'C50 H90 N4 P4 Rh2'
_chemical_formula_sum            'C50 H90 N4 P4 Rh2'
_chemical_formula_weight         1076.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.663(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.2036(17)
_cell_length_b                   11.4050(7)
_cell_length_c                   33.691(2)
_cell_measurement_temperature    123(2)
_cell_volume                     10815.0(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            70661
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         74.647
_diffrn_reflns_theta_min         2.628
_exptl_absorpt_coefficient_mu    6.315
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.7800.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.834
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         10707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+66.5605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                8668
_reflns_number_total             10707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00305_si_002.cif
_cod_data_source_block           UMN15009_compound5
_cod_original_cell_volume        10814.9(12)
_cod_database_code               4346108
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.435
_shelx_res_checksum              76289
_shelx_hkl_checksum              65659