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_1558983
_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         'C69 H99 Co N4 O P3 Zr, C24 H20 B'
_chemical_formula_sum            'C93 H119 B Co N4 O P3 Zr'
_chemical_formula_weight         1562.79
_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             2019-10-09
_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                87.197(4)
_cell_angle_beta                 83.485(3)
_cell_angle_gamma                77.866(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7732(8)
_cell_length_b                   12.9749(8)
_cell_length_c                   28.770(2)
_cell_measurement_reflns_used    9699
_cell_measurement_temperature    200
_cell_measurement_theta_max      24.773
_cell_measurement_theta_min      2.367
_cell_volume                     4629.9(5)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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      200
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            107672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         1.425
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0724 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.8482. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             1660
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether, CH2Cl2'
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         18874
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+2.0426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14425
_reflns_number_total             18874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04229c2.cif
_cod_data_source_block           '[5][BPh4]'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1558983
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.911
_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
 C50-C49
 2.5 with sigma of 0.02
 C49-C48
 2.5 with sigma of 0.02
 C48-C50
 2.5 with sigma of 0.02
 C50A-C48A
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C49) = Uanis(C48) = Uanis(C50)
Uanis(C88) = Uanis(C88A) = Uanis(C89A) = Uanis(C89) = Uanis(C90) = Uanis(C90A)
= Uanis(C91A) = Uanis(C91) = Uanis(C92A) = Uanis(C92) = Uanis(C93) = Uanis(C93A)
Uanis(C49A) = Uanis(C48) = Uanis(C48A) = Uanis(C49) = Uanis(C50A) = Uanis(C50)
4. Others
 Sof(C88A)=Sof(C89A)=Sof(H3AE)=Sof(C90A)=Sof(H4AE)=Sof(C91A)=Sof(H5AB)=
 Sof(C92A)=Sof(H6AB)=Sof(C93A)=Sof(H7AB)=1-FVAR(1)
 Sof(C88)=Sof(C89)=Sof(H02Q)=Sof(C90)=Sof(H02S)=Sof(C91)=Sof(H02R)=Sof(C92)=
 Sof(H02T)=Sof(C93)=Sof(H02U)=FVAR(1)
 Sof(C48A)=Sof(H3AB)=Sof(H3AC)=Sof(H3AD)=Sof(C49A)=Sof(H4AB)=Sof(H4AC)=
 Sof(H4AD)=Sof(C50A)=Sof(H2AB)=Sof(H2AC)=Sof(H2AD)=1-FVAR(2)
 Sof(C48)=Sof(H4A)=Sof(H4C)=Sof(H4B)=Sof(C49)=Sof(H3B)=Sof(H3A)=Sof(H3C)=
 Sof(C50)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C10(H00N), C13(H00W), C25(H00K), C28(H00S), C40(H00H), C43(H00G)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H026), C7(H02G), C19(H00U), C22(H00R), C34(H0BA), C37(H2BA), C53(H010),
 C54(H4AA), C55(H1BA), C56(H022), C57(H016), C59(H00T), C60(H2AA), C61(H027),
 C62(H6AA), C63(H00Q), C65(H01Y), C66(H029), C67(H5AA), C68(H7AA), C69(H013),
 C71(H00V), C72(H4BA), C73(H02X), C74(H6BA), C75(H02), C77(H025), C78(H02Y),
 C79(H02W), C80(H023), C81(H015), C83(H021), C84(H02Z), C85(H02V), C86(H5BA),
 C87(H3BA), C89A(H3AE), C90A(H4AE), C91A(H5AB), C92A(H6AB), C93A(H7AB),
 C89(H02Q), C90(H02S), C91(H02R), C92(H02T), C93(H02U)
5.c Fitted hexagon refined as free rotating group:
 C88A(C89A,C90A,C91A,C92A,C93A)
5.d Idealised Me refined as rotating group:
 C3(H01V,H01W,H01X), C6(H02N,H02O,H02P), C9(H8AA,HJ,HK), C11(H3AA,HH,HI),
 C12(H02A,H02B,H02C), C14(H1AA,HF,HG), C15(H01S,H01T,H01U), C18(H00A,H00B,H00C),
  C21(H02H,H02I,H02J), C24(H01G,H01H,H01I), C26(H02D,H02E,H02F), C27(H,H01Z,HA),
  C29(H9AA,HL,HM), C30(H0AA,HD,HE), C33(H01J,H01K,H01L), C36(H02K,H02L,H02M),
 C39(H01P,H01Q,H01R), C41(H01M,H01N,H01O), C42(H01,HB,HC), C44(H01A,H01B,H01C),
 C45(H01D,H01E,H01F), C48A(H3AB,H3AC,H3AD), C49A(H4AB,H4AC,H4AD), C50A(H2AB,
 H2AC,H2AD), C48(H4A,H4C,H4B), C49(H3B,H3A,H3C), C50(H2A,H2B,H2C)
;
_shelx_res_checksum              18551
_shelx_fab_checksum              76537
_olex2_submission_special_instructions 'No special instructions were received'