Sterically encumbered β-diketonates and base metal catalysis.
Krajewski, Sebastian M.; Crossman, Aaron S.; Akturk, Eser S.; Suhrbier, Tim; Scappaticci, Steven J.; Staab, Maxwell W.; Marshak, Michael P.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10714–10722; doi:10.1039/c9dt02293g

data_7701516
_publ_section_title
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 Sterically encumbered \b-diketonates and base metal catalysis.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10714
_journal_page_last               10722
_journal_paper_doi               10.1039/c9dt02293g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C70 H86 Co O6'
_chemical_formula_sum            'C70 H86 Co O6'
_chemical_formula_weight         1082.31
_chemical_name_common            Co(Aracac)2(THF)2-cis
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-09-18 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.001(9)
_cell_length_b                   35.001
_cell_length_c                   10.840(3)
_cell_measurement_reflns_used    9750
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.297
_cell_measurement_theta_min      2.816
_cell_volume                     13280(5)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            349141
_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         27.528
_diffrn_reflns_theta_min         2.498
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0577 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.9539. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       block
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         15274
_refine_ls_number_restraints     301
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0447P)^2^+8.9718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12817
_reflns_number_total             15274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02293g2.cif
_cod_data_source_block           Coaracac2thf2-cis
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7701516
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C61A \\sim C60 \\sim C62A \\sim C62 \\sim C60A \\sim C61 \\sim C68A \\sim C68
\\sim C69 \\sim C69A: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
4. Others
 Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(H61D)=Sof(H61E)=
 Sof(H61F)=Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(1)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(1)
 Sof(H67C)=Sof(H67D)=Sof(H70C)=Sof(H70D)=Sof(C68A)=Sof(H68A)=Sof(H68B)=
 Sof(C69A)=Sof(H69A)=Sof(H69B)=1-FVAR(2)
 Sof(H67A)=Sof(H67B)=Sof(H70A)=Sof(H70B)=Sof(C69)=Sof(H69C)=Sof(H69D)=Sof(C68)=
 Sof(H68C)=Sof(H68D)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,
 H67B), C67(H67C,H67D), C70(H70A,H70B), C70(H70C,H70D), C68A(H68A,H68B),
 C69A(H69A,H69B), C69(H69C,H69D), C68(H68C,H68D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C12(H12), C14(H14), C21(H21), C23(H23),
 C33(H33), C37(H37), C38(H38), C39(H39), C43(H43), C45(H45), C52(H52), C54(H54)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C60A(H60D,H60E,H60F), C61A(H61D,H61E,H61F), C62A(H62D,H62E,H62F)
;
_olex2_submission_special_instructions 'No special instructions were received'