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_4515037
_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 Ir N6 O3, F6 P'
_chemical_formula_sum            'C56 H72 F6 Ir N6 O3 P'
_chemical_formula_weight         1214.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.386(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.527(3)
_cell_length_b                   10.6934(14)
_cell_length_c                   24.942(3)
_cell_measurement_reflns_used    835
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.79
_cell_measurement_theta_min      2.40
_cell_volume                     5535.8(13)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.5670
_diffrn_reflns_av_unetI/netI     0.5490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72636
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.694
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.509
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.368
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         9747
_refine_ls_number_restraints     620
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.3107
_refine_ls_R_factor_gt           0.0895
_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^)+(0.0454P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2790
_reflns_number_total             9747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00514_si_002.cif
_cod_data_source_block           complex_2b_18m_db21_lct139_0s
_cod_original_cell_volume        5535.7(13)
_cod_database_code               4515037
_publcif_datablock.id            {79244e61-f2b9-4dc4-8cea-b916e04bfbcc}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.569
_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. Uiso/Uaniso restraints and constraints
Uanis(C55) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
Uanis(C51) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, Ir1, N1, N2, N3, N4, N5, N6, O1, O2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1, F2, F3, F4, F5, F6, P1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28), C37(H37), C40(H40), C49(H49), C52(H52)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
4.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)
4.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              69846
_shelx_hkl_checksum              7227
_olex2_submission_special_instructions 'No special instructions were received'