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_1516553
_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
'C72 H140 B Ir2 P4, C32 H12 B F24, C6 H5 F, 0.5(C5H12)'
_chemical_formula_sum            'C112.5 H163 B2 F25 Ir2 P4'
_chemical_formula_weight         2484.26
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ac'
_symmetry_space_group_name_H-M   'P 21 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.435(3)
_cell_length_b                   17.300(4)
_cell_length_c                   20.951(4)
_cell_measurement_reflns_used    7431
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     5957(2)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13594
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    2.367
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            'very pale yellow'
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.136
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.527(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         13594
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+10.9855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                11445
_reflns_number_total             13594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00735b2.cif
_cod_data_source_block           Borohydride
_cod_database_code               1516553