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_1558987
_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         'C64 H90 Cl Co N3 O P3 Zr, 2.5(C6 H5 F)'
_chemical_formula_sum            'C79 H102.5 Cl Co F2.5 N3 O P3 Zr'
_chemical_formula_weight         1436.14
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     dual
_audit_creation_date             2019-09-19
_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                86.395(2)
_cell_angle_beta                 72.314(2)
_cell_angle_gamma                75.548(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8096(9)
_cell_length_b                   17.9356(12)
_cell_length_c                   18.3046(11)
_cell_measurement_reflns_used    9515
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.280
_cell_measurement_theta_min      2.881
_cell_volume                     3879.5(4)
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            209586
_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         28.286
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0575 before and 0.0402 after correction. The Ratio of minimum to maximum transmission is 0.9016. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       plate
_exptl_crystal_F_000             1514
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, fluorobenzene'
_exptl_crystal_size_max          0.765
_exptl_crystal_size_mid          0.406
_exptl_crystal_size_min          0.264
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         19229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+2.6259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18001
_reflns_number_total             19229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04229c2.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C79 H102.50 Cl Co F2.50 N3 O P3 Zr'
_cod_database_code               1558987
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.704
_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
 Fixed Sof: F1(0.5) C65(0.5) C66(0.5) H66(0.5) C67(0.5) H67(0.5) C68(0.5)
 H68(0.5) C69(0.5) H69(0.5) C70(0.5) H70(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C25(H25), C28(H28), C40(H40), C43(H43)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C19(H19), C22(H22), C34(H34), C37(H37), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82),
  C66(H66), C67(H67), C68(H68), C69(H69), C70(H70)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,
 H18C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C),
 C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              82548
_shelx_fab_checksum              67750
_olex2_submission_special_instructions 'No special instructions were received'