Multiple metal-bound oligomers from Ir-catalysed dehydropolymerisation of H3B·NH3 as probed by experiment and computation
Kumar, Amit; Johnson, Heather C.; Hooper, Thomas N.; Weller, Andrew S.; Algarra, Andrés G.; Macgregor, Stuart A.; Chemical Science 5 (2014) 2546–; doi:10.1039/c4sc00735b

data_1516554
_publ_section_title
;
 Multiple metal-bound oligomers from Ir-catalysed dehydropolymerisation of
 H3B&#x00B7;NH3 as probed by experiment and computation
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2546
_journal_paper_doi               10.1039/c4sc00735b
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety
'C36 H82 B3 Ir1 N3 P2, C24 H12 B1 Cl8, 2(C5 H12)'
_chemical_formula_sum            'C70 H118 B4 Cl8 Ir N3 P2'
_chemical_formula_weight         1582.76
_chemical_name_systematic        '[IrH2PCy3-trimer][BArCl]'
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             14-01-30
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                99.5231(4)
_cell_angle_beta                 98.2550(3)
_cell_angle_gamma                95.4001(3)
_cell_formula_units_Z            2
_cell_length_a                   12.73770(10)
_cell_length_b                   12.84910(10)
_cell_length_c                   25.1406(2)
_cell_measurement_reflns_used    15803
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3986.57(5)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_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  0.030
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            58065
_diffrn_reflns_theta_full        25.314
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         5.110
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.76735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.12
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1075
_refine_ls_number_reflns         18071
_refine_ls_number_restraints     140
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.0426278
_refine_ls_shift/su_mean         0.0006259
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 8.77P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0795
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0795
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                16128
_reflns_number_total             18071
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.63
_oxford_diffrn_Wilson_scale      19.97
_oxford_refine_ls_r_factor_ref   0.0438
_oxford_refine_ls_scale          0.21142(6)
_oxford_reflns_number_all        18071
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'Compound X At 10:17 on 30/ 1'
_cod_data_source_file            c4sc00735b2.cif
_cod_data_source_block           Irtrimer
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C70 H118 B4 Cl8 Ir1 N3 P2'
_cod_database_code               1516554
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT H    (    1 ,X'S)  UNTIL H    (   16 ) 
CONT B    (    1 ,X'S,U'S)  UNTIL N    (    3 ) 
CONT H    (  101 ,X'S)  UNTIL H    (  691 ) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(71) C(72) C(73) C(74) C(75) AND 
CONT C(75) C(74) C(73) C(72) C(71) 
SIMU 0.015 C(71) C(72) C(73) C(74) C(75) AND 
CONT C(75) C(74) C(73) C(72) C(71) 
DELU 0.015 C(71) C(72) C(73) C(74) C(75) AND 
CONT C(75) C(74) C(73) C(72) C(71) 
SAME C(81) C(82) C(83) C(84) C(85) AND 
CONT C(85) C(84) C(83) C(82) C(81) 
SIMU 0.015 C(81) C(82) C(83) C(84) C(85) AND 
CONT C(85) C(84) C(83) C(82) C(81) 
DELU 0.015 C(81) C(82) C(83) C(84) C(85) AND 
CONT C(85) C(84) C(83) C(82) C(81) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;