Allenylphosphonium Complexes of Rhodium and Iridium
Cade, Ian A.; Colebatch, Annie L.; Hill, Anthony F.; Willis, Anthony C.; Organometallics 33 (2014) 3198–; doi:10.1021/om500450e

data_4083596
_publ_section_title
;
 Allenylphosphonium Complexes of Rhodium and Iridium
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3198
_journal_paper_doi               10.1021/om500450e
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        local
_chemical_formula_moiety         'C58 H48 Br Ir O P3 +, P F6 -, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C59.5 H51 Br Cl3 F6 Ir O P4'
_chemical_formula_weight         1398.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-07-19
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record
;
2010-07-19 - Report on C59.5 H51 Br Cl3 F6 Ir O P4
            by Anthony C. Willis
            for Anthony F. Hill, Annie L. Colebatch

2010-07-20 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                65.5999(19)
_cell_angle_beta                 86.674(2)
_cell_angle_gamma                66.190(2)
_cell_formula_units_Z            4
_cell_length_a                   17.5245(7)
_cell_length_b                   20.0599(6)
_cell_length_c                   22.9773(8)
_cell_measurement_reflns_used    422209
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     6672.3(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement
'CRYSTALS (Betteridge et al., 2003), SQUEEZE (Spek et al., 1990)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61450
_diffrn_reflns_theta_full        25.130
_diffrn_reflns_theta_max         27.615
_diffrn_reflns_theta_min         2.563
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.867
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_refine_diff_density_max         3.72
_refine_diff_density_min         -3.81
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9593
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1360
_refine_ls_number_reflns         28789
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.0071608
_refine_ls_shift/su_mean         0.0012919
_refine_ls_structure_factor_coef Fsqd
_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: 
 28.8 39.4 19.0 4.49 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1568
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1568
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              26
_reflns_limit_k_min              -23
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                18513
_reflns_number_total             28789
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.73
_oxford_diffrn_Wilson_scale      49.41
_oxford_refine_ls_r_factor_ref   0.1005
_oxford_refine_ls_scale          0.15519(4)
_oxford_reflns_number_all        28789
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '7161127 hil1001 - relabelled'
_cod_data_source_file            om500450e_si_001.cif
_cod_data_source_block           hil1001
_cod_depositor_comments
'Adding full bibliography for 4083595--4083597.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4083596