Amidate-Ligated Complexes of Rhodium(I): A Showcase of Coordination Flexibility
Drover, Marcus W.; Schafer, Laurel L.; Love, Jennifer A.; Organometallics 34 (2015) 1783–; doi:10.1021/om501209c

data_4086023
_publ_section_title
;
 Amidate-Ligated Complexes of Rhodium(I): A Showcase of Coordination
 Flexibility
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1783
_journal_paper_doi               10.1021/om501209c
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C52 H60 N2 O2 Rh2'
_chemical_formula_sum            'C52 H60 N2 O2 Rh2'
_chemical_formula_weight         950.84
_chemical_name_systematic
'bicyclo[2.2.1]hepta-2,5-diene{N-2,6-diisopropylphenyl(t-butyl)amidato}rhodium(I) dimer'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.067(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.678(7)
_cell_length_b                   11.678(5)
_cell_length_c                   22.492(10)
_cell_measurement_reflns_used    8700
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.299
_cell_measurement_theta_min      3.712
_cell_volume                     4284(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      90
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40985
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.771
_diffrn_reflns_theta_min         1.852
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.8773
_exptl_absorpt_correction_T_min  0.7367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0651 after correction.
The Ratio of minimum to maximum transmission is 0.8397.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0265P)^2^+6.0776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5733
_reflns_number_total             6047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501209c_si_002.cif
_cod_data_source_block           mo_ls499monoc
_cod_database_code               4086023
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.775
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C20(H20), C22(H22), C24(H24), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23a,H23b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)
2.d Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C18(H18a,H18b,H18c), C19(H19a,H19b,
 H19c)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id MWD
_olex2_submission_special_instructions 'No special instructions were received'