Small Molecule Activation by Intermolecular Zr(IV)-Phosphine Frustrated Lewis Pairs.
Metters, Owen J.; Forrest, Sebastian J. K.; Sparkes, Hazel A.; Manners, Ian; Wass, Duncan F.; Journal of the American Chemical Society 138 (2016) 1994–2003; doi:10.1021/jacs.5b12536

data_4129993
_publ_section_title
;
 Small Molecule Activation by Intermolecular Zr(IV)-Phosphine Frustrated
 Lewis Pairs.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1994
_journal_page_last               2003
_journal_paper_doi               10.1021/jacs.5b12536
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'B C24 F20, C29 H41 O Zr, C6 H5 Cl1'
_chemical_formula_sum            'C59 H46 B Cl F20 O Zr'
_chemical_formula_weight         1288.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7527(3)
_cell_length_b                   18.8854(4)
_cell_length_c                   19.4012(4)
_cell_measurement_reflns_used    7328
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.992
_cell_measurement_theta_min      2.36
_cell_volume                     5396.43(19)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker Apex II kappa CCDC area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCDC 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  0.0547
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41764
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         1.383
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0611 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.8998.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         11030
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0412P)^2^+9.4517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8158
_reflns_number_total             11030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12536_si_002.cif
_cod_data_source_block           2
_cod_database_code               4129993
_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. Restrained distances
 Cl1A-C54A \\sim Cl1-C54
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim Cl1A
\\sim C54A \\sim C59A \\sim C58A \\sim C57A \\sim C56A \\sim C55A: within 1.7A
with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C55) = Uanis(C59A) = Uanis(C59) = Uanis(C55A)
4. Others
 Fixed Sof: Cl1(0.79522) C54(0.79522) C55(0.79522) H55(0.79522) C56(0.79522)
 H56(0.79522) C57(0.79522) H57(0.79522) C58(0.79522) H58(0.79522) C59(0.79522)
 H59(0.79522) Cl1A(0.20478) C54A(0.20478) C59A(0.20478) H59A(0.20478)
 C58A(0.20478) H58A(0.20478) C57A(0.20478) H57A(0.20478) C56A(0.20478)
 H56A(0.20478) C55A(0.20478) H55A(0.20478)
5.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C59A(H59A), C58A(H58A), C57A(H57A), C56A(H56A), C55A(H55A)
5.b Fitted hexagon refined as free rotating group:
 C54(C55,C56,C57,C58,C59), C54A(C59A,C58A,C57A,C56A,C55A)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              80983
_shelx_hkl_checksum              46692
_olex2_submission_special_instructions 'No special instructions were received'