Organometallic Iridium Complex Containing a Dianionic, Tridentate, Mixed Organic-Inorganic Ligand.
Bloomfield, Aaron J.; Matula, Adam J.; Mercado, Brandon Q.; Batista, Victor S.; Crabtree, Robert H.; Inorganic chemistry 55 (2016) 8121–8129; doi:10.1021/acs.inorgchem.6b01218

data_4348485
_publ_section_title
;
 Organometallic Iridium Complex Containing a Dianionic, Tridentate, Mixed
 Organic-Inorganic Ligand.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8121
_journal_page_last               8129
_journal_paper_doi               10.1021/acs.inorgchem.6b01218
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C20 H26 B3 Ir N2 O6, 2(H2 O)'
_chemical_formula_sum            'C20 H30 B3 Ir N2 O8'
_chemical_formula_weight         651.09
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.959(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3069(2)
_cell_length_b                   16.4356(3)
_cell_length_c                   15.5445(3)
_cell_measurement_reflns_used    43972
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.6440
_cell_measurement_theta_min      2.7280
_cell_volume                     2334.39(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_molecular_graphics
; 
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program 
(2009). J. Appl. Cryst., 42, 339-341. 
;
_computing_publication_material  'SHELXL-2013/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1666
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65862
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.890
_diffrn_reflns_theta_max         66.889
_diffrn_reflns_theta_min         3.953
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.501
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41o (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.000
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4139
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0669P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3464
_reflns_number_total             4139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01218_si_002.cif
_cod_data_source_block           007-16003
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4348485
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.393
_shelx_estimated_absorpt_t_max   0.656
_shelx_res_checksum              10190
_shelx_hkl_checksum              66321