Role of Hemilabile Diamine Ligands in the Amine-Directed C‒H Borylation of Arenes
Hale, Lillian V. A.; McGarry, Kathryn A.; Ringgold, Marissa A.; Clark, Timothy B.; Organometallics 34 (2015) 51–; doi:10.1021/om5007837

data_4085316
_publ_section_title
;
 Role of Hemilabile Diamine Ligands in the Amine-Directed C--H Borylation
 of Arenes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              51
_journal_paper_doi               10.1021/om5007837
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C20 H24 Cl Ir N2'
_chemical_formula_sum            'C20 H24 Cl Ir N2'
_chemical_formula_weight         520.06
_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   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                105.492(2)
_cell_angle_beta                 102.412(2)
_cell_angle_gamma                90.028(2)
_cell_formula_units_Z            4
_cell_length_a                   10.5383(10)
_cell_length_b                   12.6574(12)
_cell_length_c                   14.6343(14)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      2.19
_cell_volume                     1833.7(3)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16626
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.630
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    7.430
_exptl_absorpt_correction_T_max  0.745553
_exptl_absorpt_correction_T_min  0.332634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'twinabs 2008/2'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.184
_refine_diff_density_max         2.768
_refine_diff_density_min         -3.169
_refine_diff_density_rms         0.252
_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     440
_refine_ls_number_reflns         8566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0379
_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/[\s^2^(Fo^2^)+(0.0598P)^2^+12.4888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7672
_reflns_number_total             8464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5007837_si_002.cif
_cod_data_source_block           TwinC_0t
_cod_database_code               4085316
_shelx_estimated_absorpt_t_min   0.144
_shelx_estimated_absorpt_t_max   0.342
_exptl_absorpt_special_details
; 
details of twining from .abs file 
BASF w/esd from .lst file 
;
_shelxl_version_number           2014/6
_shelx_res_checksum              52878
_shelx_hkl_checksum              18413