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_4086025
_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         'C53 H56 N O P2 Rh'
_chemical_formula_sum            'C53 H56 N O P2 Rh'
_chemical_formula_weight         887.83
_chemical_name_systematic
'[N-(2,6-diisopropylphenyl)t-butylamidate]bis(triphenylphosphine)rhodium(I)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_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                96.647(3)
_cell_angle_beta                 103.890(3)
_cell_angle_gamma                109.960(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8229(14)
_cell_length_b                   13.5515(18)
_cell_length_c                   16.978(2)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.32
_cell_volume                     2218.1(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51650
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.550
_diffrn_reflns_theta_min         2.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.9563
_exptl_absorpt_correction_T_min  0.8941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0497 before and 0.0443 after correction.
The Ratio of minimum to maximum transmission is 0.9350.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         13582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0283P)^2^+1.1637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11774
_reflns_number_total             13582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501209c_si_002.cif
_cod_data_source_block           mo_ls525_0m_a
_cod_database_code               4086025
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
 C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51),
  C52(H52), C53(H53)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id MWD-947A
_olex2_submission_special_instructions 'No special instructions were received'