Redox chemistry and H-atom abstraction reactivity of a terminal zirconium(IV) oxo compound mediated by an appended cobalt(I) center
Thomas, Christine M.; Zhang, Hongtu; Hatzis, Gregory P.; Moore, Curtis; Dickie, Diane Amanda; Chemical Science  (2020) –; doi:10.1039/D0SC04229C

data_1558989
_publ_section_title
;
 Redox chemistry and H-atom abstraction reactivity of a terminal
 zirconium(IV) oxo compound mediated by an appended cobalt(I) center
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04229C
_journal_year                    2020
_chemical_formula_moiety         'C50 H84 Co F N4 P3 Zr, F6 P1, 2(C6 H5 F)'
_chemical_formula_sum            'C62 H94 Co F9 N4 P4 Zr'
_chemical_formula_weight         1340.44
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2020-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.377(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3643(8)
_cell_length_b                   19.0177(10)
_cell_length_c                   22.7503(11)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.282
_cell_measurement_theta_min      2.720
_cell_volume                     6618.2(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  MoSource_OSU
_diffrn_radiation_monochromator  'TRIUMPH curved--crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            327838
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0517 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.9144. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, fluorobenzene'
_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.223
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         16438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0318P)^2^+4.3011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15041
_reflns_number_total             16438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04229c2.cif
_cod_data_source_block           '[7][PF6]'
_cod_database_code               1558989
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.746
_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. Others
 Sof(F00W)=Sof(F01H)=Sof(F00H)=Sof(F00P)=Sof(P0)=Sof(F00K)=Sof(F01W)=1-FVAR(1)
 Sof(P006)=Sof(F00G)=Sof(F00J)=Sof(F00O)=Sof(F00V)=Sof(F01G)=Sof(F01V)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00I(H00I), C00K(H00K), C00Q(H00Q), C00T(H00T), C00W(H00W)
3.b Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C010(H010), C011(H011), C015(H015), C01A(H01S), C01B(H01T),
 C01Q(H0BA), C01S(H1BA), C01T(H2BA), C01W(H3BA), C020(H020), C021(H021),
 C022(H022), C025(H025), C026(H026), C028(H028)
3.c Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C012(H01A,H01B,H01C), C013(H01D,H01E,H01F), C016(H01G,
 H01H,H01I), C017(H01J,H01K,H01L), C018(H01M,H01N,H01O), C019(H01P,H01Q,H01R),
 C01D(H01U,H01V,H01W), C01E(H01X,H01Y,H), C01F(H01Z,HA,HB), C01H(H01,HC,HD),
 C01I(H0AA,HE,HF), C01J(H1AA,HG,HH), C01K(H2AA,HI,HJ), C01L(H3AA,HK,HL),
 C01M(H4AA,HM,HN), C01N(H5AA,HO,HP), C01P(H6AA,HQ,HR), C01R(H7AA,HS,HT),
 C01Y(H8AA,HU,HV), C01Z(H9AA,HW,HX), C023(H02A,H02B,H02C), C027(H02D,H02E,H02F),
  C029(H02G,H02H,H02I)
;
_shelx_res_checksum              17918
_olex2_submission_special_instructions 'No special instructions were received'