Hydroboration of carbon dioxide with catechol- and pinacolborane using an Ir-CNP* pincer complex. Water influence on the catalytic activity.
Sánchez, Práxedes; Hernández-Juárez, Martín; Rendón, Nuria; López-Serrano, Joaquín; Álvarez, Eleuterio; Paneque, Margarita; Suárez, Andrés; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16766–16776; doi:10.1039/c8dt03951h

data_7047916
_publ_section_title
;
 Hydroboration of carbon dioxide with catechol- and pinacolborane using an
 Ir-CNP* pincer complex. Water influence on the catalytic activity.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16766
_journal_page_last               16776
_journal_paper_doi               10.1039/c8dt03951h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H29 Ir N3 O P, C4 H8 O'
_chemical_formula_sum            'C36 H37 Ir N3 O2 P'
_chemical_formula_weight         766.86
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-07-16 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.875(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5322(5)
_cell_length_b                   10.5191(6)
_cell_length_c                   26.4134(12)
_cell_measurement_reflns_used    1640
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.56
_cell_measurement_theta_min      2.49
_cell_volume                     3146.6(3)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
; 
 Bruker-Nonius X8kappa APEX II CCD area detector 
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            21544
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.089
_exptl_absorpt_coefficient_mu    4.331
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_correction_T_min  0.8126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
program SADABS, Bruker (2001). 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       needle
_exptl_crystal_F_000             1528
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3769
_reflns_number_total             5648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03951h3.cif
_cod_data_source_block           2a
_cod_depositor_comments          'Adding full bibliography for 7047916.cif.'
_cod_database_code               7047916
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              96127