Reactivity of an Unsaturated Iridium(III) Phosphoramidate Complex, [Cp*Ir{κ2-N,O}][BArF4]
Drover, Marcus W.; Johnson, Heather C.; Schafer, Laurel L.; Love, Jennifer A.; Weller, Andrew S.; Organometallics 34 (2015) 3849–; doi:10.1021/acs.organomet.5b00397

data_4087605
_publ_section_title
;
 Reactivity of an Unsaturated Iridium(III) Phosphoramidate Complex,
 [Cp*Ir{\k2-N,O}][BArF4]
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3849
_journal_paper_doi               10.1021/acs.organomet.5b00397
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C32 H12 B F24, C20 H30 Ir2'
_chemical_formula_sum            'C52 H42 B F24 Ir2'
_chemical_formula_weight         1518.11
_chemical_name_systematic        '[Ir2Cp*2H3][BArF4]'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                91.0343(7)
_cell_angle_beta                 97.3543(7)
_cell_angle_gamma                98.1876(8)
_cell_formula_units_Z            2
_cell_length_a                   10.8290(2)
_cell_length_b                   12.6902(2)
_cell_length_c                   19.9820(4)
_cell_measurement_reflns_used    11577
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2693.78(9)
_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    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46294
_diffrn_reflns_theta_full        26.970
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         5.148
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.054
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         4.01
_refine_diff_density_min         -4.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         12286
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.0165210
_refine_ls_shift/su_mean         0.0005373
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 7.73P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0944
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8556
_reflns_number_total             12286
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.97
_oxford_diffrn_Wilson_scale      86.26
_oxford_refine_ls_r_factor_ref   0.0778
_oxford_refine_ls_scale          0.083226(13)
_oxford_reflns_number_all        12286
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'HCJ_020b At 9:18 on 8/ 9'
_cod_data_source_file            om5b00397_si_002.cif
_cod_data_source_block           11BARF
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C52 H42 B1 F24 Ir2'
_cod_database_code               4087605
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  63,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  73,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  83,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  93,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) H   ( 193,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 203,X'S) H   ( 202,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(47) C(52) F(220) F(230) F(240) AND 
CONT C(47) C(52) F(230) F(240) F(220) AND 
CONT C(47) C(52) F(240) F(220) F(230) AND 
CONT C(47) C(52) F(221) F(231) F(241) AND 
CONT C(47) C(52) F(231) F(241) F(221) AND 
CONT C(47) C(52) F(241) F(221) F(231) 
DELU 0.015 C(47) C(52) F(220) F(230) F(240) AND 
CONT C(47) C(52) F(230) F(240) F(220) AND 
CONT C(47) C(52) F(240) F(220) F(230) AND 
CONT C(47) C(52) F(221) F(231) F(241) AND 
CONT C(47) C(52) F(231) F(241) F(221) AND 
CONT C(47) C(52) F(241) F(221) F(231) 
SIMU 0.015 C(47) C(52) F(220) F(230) F(240) AND 
CONT C(47) C(52) F(230) F(240) F(220) AND 
CONT C(47) C(52) F(240) F(220) F(230) AND 
CONT C(47) C(52) F(221) F(231) F(241) AND 
CONT C(47) C(52) F(231) F(241) F(221) AND 
CONT C(47) C(52) F(241) F(221) F(231) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;