Ligand dynamics and protonation preferences of Rh and Ir complexes bearing an almost, but not quite, pendent base.
Morrow, T. J.; Christman, W. E.; Williams, J. Z.; Arulsamy, N.; Goroncy, A.; Hulley, E. B.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2670–2682; doi:10.1039/c7dt04259k

data_7045326
_publ_section_title
;
 Ligand dynamics and protonation preferences of Rh and Ir complexes
 bearing an almost, but not quite, pendent base.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2670
_journal_page_last               2682
_journal_paper_doi               10.1039/c7dt04259k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C23 H29 Ir N3), 2(Cl), 3(O)'
_chemical_formula_sum            'C23 H29 Cl Ir N3 O1.5'
_chemical_formula_weight         599.14
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-04 deposited with the CCDC.
2018-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                114.387(2)
_cell_angle_beta                 97.829(1)
_cell_angle_gamma                99.861(1)
_cell_formula_units_Z            4
_cell_length_a                   9.5235(2)
_cell_length_b                   15.9622(4)
_cell_length_c                   16.7580(4)
_cell_measurement_reflns_used    9175
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.31
_cell_measurement_theta_min      2.40
_cell_volume                     2224.30(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62580
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.727
_diffrn_reflns_theta_min         1.447
_exptl_absorpt_coefficient_mu    6.145
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.4852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.116
_refine_diff_density_max         7.089
_refine_diff_density_min         -3.228
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         17670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+5.6923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14202
_reflns_number_total             17670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04259k2.cif
_cod_data_source_block           tm02d
_cod_depositor_comments
'Adding full bibliography for 7045326--7045328.cif.'
_cod_original_cell_volume        2224.30(9)
_cod_original_formula_sum        'C23 H29 Cl Ir N3 O1.50'
_cod_database_code               7045326
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.226
_shelx_estimated_absorpt_t_max   0.536
_shelx_res_checksum              35804