Synthesis, NMR, and X-ray Studies of Iridium Dihydride C,N and N,P Ligand Complexes
Gruber, Stefan; Organometallics 35 (2016) 699–; doi:10.1021/acs.organomet.5b00989

data_4088286
_publ_section_title
;
 Synthesis, NMR, and X-ray Studies of Iridium Dihydride C,N and N,P Ligand
 Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              699
_journal_paper_doi               10.1021/acs.organomet.5b00989
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H12 B F24, C26 H40 Ir N O P'
_chemical_formula_sum            'C58 H52 B F24 Ir N O P'
_chemical_formula_weight         1469.01
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 101.310(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6765(11)
_cell_length_b                   18.1773(16)
_cell_length_c                   12.9092(11)
_cell_measurement_reflns_used    13084
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     2916.8(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32629
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         68.301
_diffrn_reflns_theta_min         3.491
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.46
_refine_diff_density_min         -0.90
_refine_ls_abs_structure_details 'Flack (1983), 4431 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0896
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         9506
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.0294010
_refine_ls_shift/su_mean         0.0006054
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.167 0.135 0.521E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0250
_refine_ls_wR_factor_gt          0.0249
_refine_ls_wR_factor_ref         0.0247
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                9647
_reflns_number_total             9743
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0214
_oxford_refine_ls_scale          0.10132(6)
_oxford_reflns_number_all        9695
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            om5b00989_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C58 H52 B1 F24 Ir1 N1 O1 P1'
_cod_database_code               4088286
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
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