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_1558986
_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 H85 Co I0 N4 O1 P3 Zr, C32 H12 B F24'
_chemical_formula_sum            'C82 H96.99 B Co F24 I0.01 N4 O P3 Zr'
_chemical_formula_weight         1865.05
_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   mixed
_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                73.132(2)
_cell_angle_beta                 81.938(2)
_cell_angle_gamma                89.151(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4865(8)
_cell_length_b                   15.0867(9)
_cell_length_c                   24.2764(14)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.892
_cell_measurement_theta_min      2.857
_cell_volume                     4678.5(5)
_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 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON II CPAD'
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            176079
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.902
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0518 before and 0.0423 after correction. The Ratio of minimum to maximum transmission is 0.9340. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1916
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, fluorobenzene'
_exptl_crystal_size_max          0.744
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.326
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         22290
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0416P)^2^+3.8073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20062
_reflns_number_total             22290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04229c2.cif
_cod_data_source_block           '[9][BArF4]'
_cod_database_code               1558986
_shelx_shelxl_version_number     2018/1
_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, All O(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.01
 Zr1-H1
 2.7 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(I1)
4. Others
 Sof(I1)=1-FVAR(1)
 Sof(O1)=Sof(H1)=FVAR(1)
 Sof(F25A)=Sof(F26A)=Sof(F27A)=1-FVAR(2)
 Sof(F25)=Sof(F26)=Sof(F27)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C25(H25), C28(H28), C39(H39), C42(H42)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C19(H19), C22(H22), C34(H34), C37(H37), C51(H51), C54(H54),
 C57(H57), C59(H59), C62(H62), C65(H65), C67(H67), C70(H70), C73(H73), C75(H75),
  C78(H78), C81(H81)
5.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), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              47995
_shelx_fab_checksum              22397
_olex2_submission_special_instructions 'No special instructions were received'