An optically pure P‒alkene-ligated Ir^I^ complex
Linden, Anthony; Dorta, Romano; Acta Crystallographica Section C 66 (2010) m290–m293; doi:10.1107/S0108270110036413

data_2017812
_publ_section_title
;
 An optically pure P--alkene-ligated Ir^I^ complex
;
_journal_coeditor_code           FG3194
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m290
_journal_page_last               m293
_journal_paper_doi               10.1107/S0108270110036413
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ir Cl (C34 H22 N O2 P)2] , C6 H6 , C5 H12'
_chemical_formula_moiety         'C68 H44 Cl Ir N2 O4 P2 , C6 H6 , C5 H12'
_chemical_formula_sum            'C79 H62 Cl Ir N2 O4 P2'
_chemical_formula_weight         1392.97
_chemical_name_systematic
;
(<i>P</i>)-chloridobis[(<i>S</i>)-(+)-5-(3,5-dioxa-4-
phosphacyclohepta[2,1-<i>a</i>;3,4-<i>a</i>']dinaphthalen-4-yl)-
dibenz[<i>b</i>,<i>f</i>]azepine]iridium(I)--benzene--pentane (1/1/1)
;
_space_group_IT_number           4
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7487(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.27160(10)
_cell_length_b                   12.69440(10)
_cell_length_c                   23.6689(2)
_cell_measurement_reflns_used    281047
_cell_measurement_temperature    160.0(10)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     6298.19(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
;
DENZO-SMN (Otwinowski & Minor, 1997) and SCALEPACK (Otwinowski & Minor,
1997)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF94 (Beurskens <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      160.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w scans with \k offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            99162
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.064
_refine_ls_abs_structure_details
'Flack & Bernardinelli (1999, 2000), with 10122 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.018(3)
_refine_ls_extinction_coef       0.00036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1610
_refine_ls_number_reflns         21762
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0338P)^2^+7.9338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                20907
_reflns_number_total             21763
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3194.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2017812
_cod_database_fobs_code          2017812