Diverse Coordination Modes of Bidentate COC and Tridentate CNC Ligands Comprising 1,2,3-Triazol-5-ylidenes
Tolley, Lewis C.; Strydom, Ian; Louw, Wynand J.; Fernandes, Manuel A.; Bezuidenhout, Daniela I.; Guisado-Barrios, Gregorio; ACS Omega 4 (2019) 6360–; doi:10.1021/acsomega.9b00514

data_4515040
_publ_section_title
;
 Diverse Coordination Modes of Bidentate COC and Tridentate CNC Ligands
 Comprising 1,2,3-Triazol-5-ylidenes
;
_journal_issue                   4
_journal_name_full               'ACS Omega'
_journal_page_first              6360
_journal_paper_doi               10.1021/acsomega.9b00514
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety
;
C70 H96 N7 Rh2, F6 P, 3(C H2 Cl2), [+ disordered mix of toluene and DCM solvent]
;
_chemical_formula_sum            'C73 H102 Cl6 F6 N7 P Rh2'
_chemical_formula_weight         1641.10
_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     dual
_audit_creation_date             2018-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                81.880(6)
_cell_angle_beta                 85.642(6)
_cell_angle_gamma                86.607(6)
_cell_formula_units_Z            2
_cell_length_a                   12.4173(11)
_cell_length_b                   16.7357(16)
_cell_length_c                   20.3867(18)
_cell_measurement_reflns_used    8155
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.31
_cell_volume                     4177.0(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0858
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            59766
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.011
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_correction_T_min  0.8040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0834 before and 0.0687 after correction. The Ratio of minimum to maximum transmission is 0.8530. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.241
_refine_diff_density_max         2.778
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         14704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.1040
_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^)+(0.0580P)^2^+78.8049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9863
_reflns_number_total             14704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00514_si_002.cif
_cod_data_source_block           complex_6_18m_db12_lct135c_0s_sq
_cod_database_code               4515040
_publcif_datablock.id            {b45dd167-bc30-4e7c-9d18-bc4cd1080fa0}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.835
_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:
 C13(H13), C16(H16), C25(H25), C28(H28), C37(H37), C40(H40), C49(H49),
 C52(H52), C55(H55), C56(H56), C59(H59), C60(H60), C63(H63), C64(H64), C67(H67),
  C68(H68)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C57(H57A,H57B), C58(H58A,H58B), C61(H61A,H61B),
 C62(H62A,H62B), C65(H65A,H65B), C66(H66A,H66B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23), C33(H33), C34(H34),
 C35(H35), C45(H45), C46(H46), C47(H47)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              4524
_shelx_hkl_checksum              81551
_shelx_fab_checksum              8126
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'