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_4515036
_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         'C56 H72 N6 O3 Rh, F6 P'
_chemical_formula_sum            'C56 H72 F6 N6 O3 P Rh'
_chemical_formula_weight         1125.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.722(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5202(11)
_cell_length_b                   10.7072(5)
_cell_length_c                   24.8940(13)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.20
_cell_volume                     5521.5(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex II'
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            209908
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.777
_diffrn_reflns_theta_min         2.182
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) 
was 0.1266 before and 0.0451 after correction. The Ratio of minimum to 
maximum transmission is 0.9670. The \l/2 correction factor is Not present.'
;
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       thick-needle
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.437(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1406
_refine_ls_number_reflns         23488
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0270P)^2^+2.5385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                21329
_reflns_number_total             23488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00514_si_002.cif
_cod_data_source_block           complex_2a_mo_isd0015_0m
_cod_database_code               4515036
_publcif_datablock.id            {75adf253-b591-4376-8fe6-f80d6edf8e61}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.858
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.563(14)
 0.437(14)
2. 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
3. Restrained distances
 C93-C94 \\sim C93-C94A \\sim C93-C95 \\sim C93-C95A
 with sigma of 0.02
 C94-C95 \\sim C94A-C95A
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C93, C94, C95
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C93, C94A, C95A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F7, F8, F9, F10, F11, F12, P2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, F8, P2, F9A, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(H93A)=Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=Sof(C95A)=Sof(H95D)=
 Sof(H95E)=Sof(H95F)=1-FVAR(2)
 Sof(H93)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=Sof(C95)=Sof(H95A)=Sof(H95B)=
 Sof(H95C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28), C37(H37), C40(H40), C49(H49),
 C52(H52), C69(H69), C72(H72), C81(H81), C84(H84), C93(H93), C93(H93A),
 C96(H96), C105(H105), C108(H108)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C59(H59A,H59B), C60(H60A,H60B)
6.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), C65(H65), C66(H66), C67(H67), C77(H77),
  C78(H78), C79(H79), C89(H89), C90(H90), C91(H91), C101(H101), C102(H102),
 C103(H103)
6.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), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C),
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C94(H94A,H94B,H94C), C95(H95A,H95B,
 H95C), C94A(H94D,H94E,H94F), C95A(H95D,H95E,H95F), C97(H97A,H97B,H97C),
 C98(H98A,H98B,H98C), C106(H10A,H10B,H10C), C107(H10D,H10E,H10F), C109(H10G,
 H10H,H10I), C110(H11A,H11B,H11C)
;
_shelx_res_checksum              14747
_shelx_hkl_checksum              75394
_olex2_submission_special_instructions 'No special instructions were received'