#------------------------------------------------------------------------------
#$Date: 2024-08-05 20:34:14 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293713 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/31/7133175.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133175
loop_
_publ_author_name
'Demchuk, Mitchell J.'
'Zurakowski, Joseph A.'
'Drover, Marcus W.'
_publ_section_title
;
 Tridentate κ³-P,P,C iridium
 complexes: influence of ligand saturation on intramolecular C-H bond
 activation.
;
_journal_issue                   59
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7566
_journal_page_last               7569
_journal_paper_doi               10.1039/d4cc01435a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C25 H49 Ir P2'
_chemical_formula_sum            'C25 H49 Ir P2'
_chemical_formula_weight         603.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-11-30 deposited with the CCDC.	2024-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.8681(5)
_cell_length_b                   14.8775(4)
_cell_length_c                   38.0030(10)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.40
_cell_volume                     10102.4(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_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       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            578338
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.336
_diffrn_reflns_theta_min         1.860
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.423
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.7783.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         6.372
_refine_diff_density_min         -3.688
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         12555
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0540
_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/[σ²(Fo²)+(0.0116P)²+144.8500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10125
_reflns_number_total             12555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc01435a3.cif
_cod_data_source_block           final360
_cod_depositor_comments
'Adding full bibliography for 7133173--7133175.cif.'
_cod_database_code               7133175
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.562
_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. Restrained distances
 C10-C13 \\sim C10-C13A
 with sigma of 0.02
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C18-C25 \\sim C18A-C25A
 with sigma of 0.02
 C23-C22 \\sim C23A-C22A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
 C25-C24 \\sim C25A-C24A
 with sigma of 0.02
 C10-C12 \\sim C10-C12A
 with sigma of 0.02
 C22-C21 \\sim C22A-C21A
 with sigma of 0.02
 C23-C25 \\sim C23A-C25A
 with sigma of 0.04
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 C23-C21 \\sim C23A-C21A
 with sigma of 0.04
 C22-C20 \\sim C22A-C20A
 with sigma of 0.04
 Ir1-C19 \\sim Ir1-C19A
 with sigma of 0.04
 Ir1-C18 \\sim Ir1-C18A
 with sigma of 0.04
 Ir1-C23 \\sim Ir1-C23A
 with sigma of 0.04
 Ir1-C25 \\sim Ir1-C25A
 with sigma of 0.04
 Ir1-C22 \\sim Ir1-C22A
 with sigma of 0.04
 Ir1-C20 \\sim Ir1-C20A
 with sigma of 0.04
 Ir1-C21 \\sim Ir1-C21A
 with sigma of 0.04
 Ir1-C24 \\sim Ir1-C24A
 with sigma of 0.04
 C19-C25 \\sim C19A-C25A
 with sigma of 0.04
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C10-C11 \\sim C10-C11A
 with sigma of 0.02
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C18-C24 \\sim C18A-C24A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C19) = Uanis(C19A) = Uanis(C20) = Uanis(C20A) = Uanis(C21A) = Uanis(C21)
= Uanis(C22A) = Uanis(C22) = Uanis(C23A) = Uanis(C23) = Uanis(C24A) =
Uanis(C24) = Uanis(C25A) = Uanis(C25) = Uanis(C18) = Uanis(C18A)
Uanis(C13) = Uanis(C13A) = Uanis(C12) = Uanis(C12A) = Uanis(C11A) = Uanis(C11)
4. Others
 Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=
 Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=1-FVAR(1)
 Sof(C19)=Sof(H19)=Sof(C18)=Sof(H18)=Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(C22)=Sof(H22)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C24)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(2)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C43(H43), C44(H44), C19(H19), C48(H48), C18(H18), C47(H47), C23(H23),
 C22(H22), C19A(H19A), C18A(H18A), C22A(H22A), C23A(H23A)
5.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C30(H30A,H30B), C29(H29A,H29B), C5(H5A,H5B), C26(H26A,H26B),
 C28(H28A,H28B), C45(H45A,H45B), C4(H4A,H4B), C50(H50A,H50B), C1(H1A,H1B),
 C2(H2A,H2B), C25(H25A,H25B), C3(H3A,H3B), C46(H46A,H46B), C49(H49A,H49B),
 C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B), C20A(H20C,H20D), C21A(H21C,
 H21D), C24A(H24C,H24D), C25A(H25C,H25D)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C16(H16A,H16B,H16C), C42(H42A,H42B,
 H42C), C36(H36A,H36B,H36C), C7(H7A,H7B,H7C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C37(H37A,H37B,H37C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C),
  C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C11A(H11D,H11E,
 H11F), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F)
;
