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_4086024
_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         'C55 H52 N O P2 Rh0.98'
_chemical_formula_sum            'C55 H52 N O P2 Rh'
_chemical_formula_weight         907.82
_chemical_name_systematic
'[N-(2,6-diisopropylphenyl)phenylamidate]bis(triphenylphosphine)rhodium(I)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.822(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.070(2)
_cell_length_b                   24.216(4)
_cell_length_c                   17.107(4)
_cell_measurement_reflns_used    4925
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.015
_cell_measurement_theta_min      2.277
_cell_volume                     4569.7(15)
_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      90.0
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_laue_measured_fraction_full 0.946
_diffrn_reflns_laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22708
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.107
_diffrn_reflns_theta_min         1.461
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0500 before and 0.0427 after correction.
 The Ratio of minimum to maximum transmission is 0.82.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0730 before and 0.0534 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 44795 reflections, Rint = 0.0650
 (13943 with I > 3sig(I), Rint = 0.0409)
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         22708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+3.0588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17892
_reflns_number_total             22708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501209c_si_002.cif
_cod_data_source_block           ls548
_cod_original_cell_volume        4569.5(16)
_cod_database_code               4086024
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.880
_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:
 C14(H14), C17(H17)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47),
  C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
2.c 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_special_instructions 'No special instructions were received'