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_4129995
_publ_section_title
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 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, C23 H29 O2 Zr, C6 H5 Cl'
_chemical_formula_sum            'C53 H34 B Cl F20 O2 Zr'
_chemical_formula_weight         1220.28
_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             2014-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                74.9625(9)
_cell_angle_beta                 66.3765(8)
_cell_angle_gamma                89.8892(9)
_cell_formula_units_Z            2
_cell_length_a                   13.3376(2)
_cell_length_b                   13.8210(3)
_cell_length_c                   14.9684(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.71
_cell_volume                     2425.17(8)
_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      100.00
_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 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  0.0185
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44859
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.950
_diffrn_reflns_theta_min         1.536
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0449 before and 0.0320 after correction.
The Ratio of minimum to maximum transmission is 0.8967.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         11650
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+1.8455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10557
_reflns_number_total             11650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12536_si_002.cif
_cod_data_source_block           Cp2Zr
_cod_database_code               4129995
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C20 \\sim O2-C20A \\sim O2-C23A \\sim O2-C23
 with sigma of 0.01
 C21-C20 \\sim C21A-C20A \\sim C23A-C22A \\sim C23-C22
 with sigma of 0.01
 C22A-C21A \\sim C22-C21
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C20 \\sim C20A \\sim C21A \\sim C21 \\sim C22 \\sim C22A \\sim C23 \\sim C23A:
within 1.7A with sigma of 0.003 and sigma for terminal atoms of 0.006
4. Others
 Fixed Sof: C20(0.66324) H20A(0.66324) H20B(0.66324) C21(0.66324)
 H21A(0.66324) H21B(0.66324) C22(0.66324) H22A(0.66324) H22B(0.66324)
 C23(0.66324) H23A(0.66324) H23B(0.66324) C22A(0.33676) H22C(0.33676)
 H22D(0.33676) C21A(0.33676) H21C(0.33676) H21D(0.33676) C20A(0.33676)
 H20C(0.33676) H20D(0.33676) C23A(0.33676) H23C(0.33676) H23D(0.33676)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C22A(H22C,
 H22D), C21A(H21C,H21D), C20A(H20C,H20D), C23A(H23C,H23D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C13(H13), C15(H15), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
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_shelx_res_checksum              14553
_shelx_hkl_checksum              88156
_olex2_submission_special_instructions 'No special instructions were received'