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_7701519
_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         'C69.54 H84.62 Co O6, 0.46(C H3)'
_chemical_formula_sum            'C70 H86 Co O6'
_chemical_formula_weight         1082.31
_chemical_name_common            Co(Aracac)2(THF)2-trans
_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     iterative
_audit_creation_date             2016-12-14
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2018-09-18 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                105.24(5)
_cell_angle_beta                 100.50(4)
_cell_angle_gamma                116.15(4)
_cell_formula_units_Z            1
_cell_length_a                   11.716(11)
_cell_length_b                   12.487(13)
_cell_length_c                   12.734(13)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    134(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.611
_cell_volume                     1515(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      134.47
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43917
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.004
_diffrn_reflns_theta_min         2.621
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0651 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.9234.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       Block
_exptl_crystal_F_000             581
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7269
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6261
_reflns_number_total             7269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02293g2.cif
_cod_data_source_block           Coaracac2thf2-trans
_cod_database_code               7701519
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Same fragment restrains
{C29, C30, C31} sigma for 1-2: 0.02, 1-3: 0.04
as
{C29A, C30A, C31A}
{C29, C30, C31} sigma for 1-2: 0.02, 1-3: 0.04
as
{C29B, C30B, C31B}
{C29, C30, C31} sigma for 1-2: 0.02, 1-3: 0.04
as
{C29C, C30C, C31C}
3. Others
 1*[Sof(C29)+Sof(H29A)+Sof(H29B)+Sof(H29C)+Sof(C30)+Sof(H30A)+Sof(H30B)+
 Sof(H30C)+Sof(C31)+Sof(H31A)+Sof(H31B)+Sof(H31C)]+1*[Sof(C29A)+Sof(H29D)+
 Sof(H29E)+Sof(H29F)+Sof(C30A)+Sof(H30D)+Sof(H30E)+Sof(H30F)+Sof(C31A)+
 Sof(H31D)+Sof(H31E)+Sof(H31F)]+1*[Sof(C29B)+Sof(H29J)+Sof(H29K)+Sof(H29L)+
 Sof(C30B)+Sof(H30G)+Sof(H30H)+Sof(H30I)+Sof(C31B)+Sof(H31G)+Sof(H31H)+
 Sof(H31I)]+1*[Sof(C29C)+Sof(H29G)+Sof(H29H)+Sof(H29I)+Sof(C30C)+Sof(H30J)+
 Sof(H30K)+Sof(H30L)+Sof(C31C)+Sof(H31J)+Sof(H31K)+Sof(H31L)]=1 with esd of
 0.0001
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=FVAR(2)
 Sof(C29B)=Sof(H29J)=Sof(H29K)=Sof(H29L)=Sof(C30B)=Sof(H30G)=Sof(H30H)=
 Sof(H30I)=Sof(C31B)=Sof(H31G)=Sof(H31H)=Sof(H31I)=FVAR(3)
 Sof(C29C)=Sof(H29G)=Sof(H29H)=Sof(H29I)=Sof(C30C)=Sof(H30J)=Sof(H30K)=
 Sof(H30L)=Sof(C31C)=Sof(H31J)=Sof(H31K)=Sof(H31L)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C12(H12), C14(H14), C21(H21), C23(H23)
4.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), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F),
 C31A(H31D,H31E,H31F), C29B(H29J,H29K,H29L), C30B(H30G,H30H,H30I), C31B(H31G,
 H31H,H31I), C29C(H29G,H29H,H29I), C30C(H30J,H30K,H30L), C31C(H31J,H31K,H31L)
;
_olex2_submission_special_instructions 'No special instructions were received'