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#$Date: 2021-11-04 16:36:26 +0200 (Thu, 04 Nov 2021) $
#$Revision: 270302 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/91/7129199.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_7129199
loop_
_publ_author_name
'Shanahan, J. P.'
'Moore, C. M.'
'Kampf, Jeff W.'
'Szymczak, N. K.'
_publ_section_title
;
Modulation of H+/H- exchange in iridium-hydride
2-hydroxypyridine complexes by remote Lewis acids.
;
_journal_issue 88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first 11705
_journal_page_last 11708
_journal_paper_doi 10.1039/d1cc04778g
_journal_volume 57
_journal_year 2021
_chemical_formula_moiety
;
2(C51 H42 Ir N3 O2 P2), (C4 H10 O), 1.5(C H2 Cl2) [+ solvent]
;
_chemical_formula_sum 'C53.75 H48.5 Cl1.5 Ir N3 O2.5 P2'
_chemical_formula_weight 1083.77
_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'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual-space
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_audit_update_record
;
2021-08-17 deposited with the CCDC. 2021-10-19 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 103.5510(10)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 15.95100(10)
_cell_length_b 27.4111(2)
_cell_length_c 23.76380(10)
_cell_measurement_reflns_used 66886
_cell_measurement_temperature 85(2)
_cell_measurement_theta_max 73.2190
_cell_measurement_theta_min 2.4840
_cell_volume 10101.10(11)
_computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature 85(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.1057
_diffrn_reflns_av_unetI/netI 0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 34
_diffrn_reflns_limit_k_min -34
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 302176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.135
_diffrn_reflns_theta_min 3.037
_diffrn_source 'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu 6.784
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.58578
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.425
_exptl_crystal_description needle
_exptl_crystal_F_000 4356
_exptl_crystal_size_max 0.060
_exptl_crystal_size_mid 0.020
_exptl_crystal_size_min 0.020
_refine_diff_density_max 2.045
_refine_diff_density_min -1.941
_refine_diff_density_rms 0.139
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 1194
_refine_ls_number_reflns 20398
_refine_ls_number_restraints 45
_refine_ls_restrained_S_all 1.039
_refine_ls_R_factor_all 0.0550
_refine_ls_R_factor_gt 0.0485
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+36.5240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1341
_refine_ls_wR_factor_ref 0.1406
_reflns_Friedel_coverage 0.000
_reflns_number_gt 17811
_reflns_number_total 20398
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d1cc04778g2.cif
_cod_data_source_block cm4119_sq
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C53.75 H48.50 Cl1.50 Ir N3 O2.50 P2'
_cod_database_code 7129199
_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_min 0.686
_shelx_estimated_absorpt_t_max 0.876
_shelx_res_file
;
TITL cm4119_a.res in P2(1)/n
cm4119_sq.res
created by SHELXL-2018/3 at 13:01:49 on 12-Mar-2021
CELL 1.54184 15.9510 27.4111 23.7638 90.000 103.551 90.000
ZERR 8.000 0.0001 0.0002 0.0001 0.000 0.001 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N O P Cl Ir
UNIT 430 388 24 20 16 12 8
REM Old TITL cm4119 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.093, Rweak 0.004, Alpha 0.049
REM