Catalytic Dehydrocoupling of Amine‒Boranes using Cationic Zirconium(IV)‒Phosphine Frustrated Lewis Pairs
Metters, Owen J.; Flynn, Stephanie R.; Dowds, Christiana K.; Sparkes, Hazel A.; Manners, Ian; Wass, Duncan F.; ACS Catalysis 6 (2016) 6601–; doi:10.1021/acscatal.6b02211

data_4513945
_publ_section_title
;
 Catalytic Dehydrocoupling of Amine--Boranes using Cationic
 Zirconium(IV)--Phosphine Frustrated Lewis Pairs
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              6601
_journal_paper_doi               10.1021/acscatal.6b02211
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C36 H51 N2 O Zr, B C24 F20'
_chemical_formula_sum            'C60 H51 B F20 N2 O Zr'
_chemical_formula_weight         1298.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1305(6)
_cell_length_b                   10.7085(4)
_cell_length_c                   29.9187(10)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.34
_cell_volume                     5488.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            95934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.962
_diffrn_reflns_theta_min         1.361
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0783 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.8066.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       plate
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 4746 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         13181
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+3.2863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11162
_reflns_number_total             13181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b02211_si_002.cif
_cod_data_source_block           S1
_cod_depositor_comments
'Adding full bibliography for 4513943--4513945.cif.'
_cod_database_code               4513945
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C30(H30), C31(H31), C33(H33), C34(H34)
2.c Idealised Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              34276
_shelx_hkl_checksum              2570
_olex2_submission_special_instructions 'No special instructions were received'