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_4129997
_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         'C55 H62 O P Zr, B C24 F20'
_chemical_formula_sum            'C79 H62 B F20 O P Zr'
_chemical_formula_weight         1540.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                73.594(2)
_cell_angle_beta                 74.388(2)
_cell_angle_gamma                82.392(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6964(4)
_cell_length_b                   15.2765(5)
_cell_length_c                   19.2500(6)
_cell_measurement_reflns_used    7766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.24
_cell_volume                     3443.1(2)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_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  0.0806
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63814
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.957
_diffrn_reflns_theta_min         1.553
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0645 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.8549.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         16537
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+1.5622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11093
_reflns_number_total             16537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12536_si_002.cif
_cod_data_source_block           2c
_cod_database_code               4129997
_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
 C15A-C11A \\sim C15-C11 \\sim C12-C11 \\sim C12A-C11A \\sim C13-C12 \\sim
C13A-C12A \\sim C14-C13 ~
 C14A-C13A \\sim C15-C14 \\sim C15A-C14A
 with sigma of 0.01
 C17A-C12A \\sim C18-C13 \\sim C18A-C13A \\sim C19-C14 \\sim C19A-C14A \\sim
C20-C15 \\sim C20A-C15A ~
 C16-C11 \\sim C16A-C11A \\sim C17-C12
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C11, C15, C16, C20, C11A, C14A, C15A, C16A, C19A, C20A, C12, C13, C14, C17,
 C18, C19, C12A, C13A, C17A, C18A
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4. Others
 Fixed Sof: C11(0.80516) C12(0.80516) C13(0.80516) C14(0.80516) C15(0.80516)
 C16(0.80516) H16A(0.80516) H16B(0.80516) H16C(0.80516) C17(0.80516)
 H17A(0.80516) H17B(0.80516) H17C(0.80516) C18(0.80516) H18A(0.80516)
 H18B(0.80516) H18C(0.80516) C19(0.80516) H19A(0.80516) H19B(0.80516)
 H19C(0.80516) C20(0.80516) H20A(0.80516) H20B(0.80516) H20C(0.80516)
 C11A(0.19484) C12A(0.19484) C13A(0.19484) C14A(0.19484) C15A(0.19484)
 C16A(0.19484) H16D(0.19484) H16E(0.19484) H16F(0.19484) C17A(0.19484)
 H17D(0.19484) H17E(0.19484) H17F(0.19484) C18A(0.19484) H18D(0.19484)
 H18E(0.19484) H18F(0.19484) C19A(0.19484) H19D(0.19484) H19E(0.19484)
 H19F(0.19484) C20A(0.19484) H20D(0.19484) H20E(0.19484) H20F(0.19484)
5.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36),
 C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
5.b 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), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F),
 C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              236
_shelx_hkl_checksum              63119
_olex2_submission_special_instructions 'No special instructions were received'