Synthesis of iridium complexes bearing {o-(Ph(2)P)C(6)H(4)}(3)E type (E = Si, Ge, and Sn) ligand and evaluation of electron donating ability of group 14 elements E.
Kameo, Hajime; Ishii, Sho; Nakazawa, Hiroshi; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8290–8296; doi:10.1039/c2dt30546a

data_7019523
_publ_section_title
;
 Synthesis of iridium complexes bearing {o-(Ph(2)P)C(6)H(4)}(3)E type (E =
 Si, Ge, and Sn) ligand and evaluation of electron donating ability of
 group 14 elements E.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8290
_journal_page_last               8296
_journal_paper_doi               10.1039/c2dt30546a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C55 H45 Ir O P3, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C57 H49 B Cl4 F4 Ir O P3'
_chemical_formula_weight         1263.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.837(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3525(6)
_cell_length_b                   23.4548(9)
_cell_length_c                   39.060(2)
_cell_measurement_reflns_used    26930
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0191
_cell_volume                     11114.9(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
scan:
Number of images: 1800
Slice: -80.0000 - 100.0000
Image width: 0.1000
Exp time: 7.0000
Rotation axis: Phi
Omega: 0.0000
Chi: 0.0000
Phi: 0.0000
XTD: 55.2404
2theta: 24.8829
scan:
Number of images: 600
Slice: -15.0000 - 45.0000
Image width: 0.1000
Exp time: 7.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 0.0000
XTD: 55.2404
2theta: 24.8829
scan:
Number of images: 600
Slice: -15.0000 - 45.0000
Image width: 0.1000
Exp time: 7.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 90.0000
XTD: 55.2404
2theta: 24.8829
scan:
Number of images: 600
Slice: -15.0000 - 45.0000
Image width: 0.1000
Exp time: 7.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 180.0000
XTD: 55.2404
2theta: 24.8829
scan:
Number of images: 600
Slice: -15.0000 - 45.0000
Image width: 0.1000
Exp time: 7.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 270.0000
XTD: 55.2404
2theta: 24.8829

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81351
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.02
_diffrn_source_current           250.0000
_diffrn_source_power             15.0000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_T_max  0.6109
_exptl_absorpt_correction_T_min  0.4480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5040
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.975
_refine_diff_density_min         -1.898
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1265
_refine_ls_number_reflns         24591
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+127.7649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                21538
_reflns_number_total             24591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30546a.txt
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        11114.8(9)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7019523