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_7701518
_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 Ni O6'
_chemical_formula_sum            'C70 H86 Ni O6'
_chemical_formula_weight         1082.09
_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             2018-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_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                   34.764(4)
_cell_length_b                   34.764(4)
_cell_length_c                   10.7447(14)
_cell_measurement_reflns_used    9217
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.507
_cell_measurement_theta_min      2.838
_cell_volume                     12985(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            434646
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.559
_diffrn_reflns_theta_min         2.304
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0439 before and 0.0420 after correction. The Ratio of minimum to maximum transmission is 0.9626. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.258
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         19904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+7.2060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16549
_reflns_number_total             19904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02293g2.cif
_cod_data_source_block           niaracac2thf2
_cod_original_cell_volume        12986(3)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7701518
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.893
_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.a Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C91(H91A,H91B), C92(H92A,H92B), C94(H94A,H94B), C93(H93A,
 H93B), C83(H83A,H83B), C81(H81A,H81B), C82(H82A,H82B)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C46(H46), C47(H47), C2(H2), C48(H48), C61(H61), C54(H54), C63(H63),
 C52(H52), C23(H23), C14(H14), C12(H12), C6(H6), C21(H21), C8(H8), C7(H7)
2.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C18(H18A,H18B,H18C), C58(H58A,H58B,H58C), C65(H65A,H65B,
 H65C), C56(H56A,H56B,H56C), C25(H25A,H25B,H25C), C57(H57A,H57B,H57C), C27(H27A,
 H27B,H27C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C70(H70A,H70B,H70C),
 C29(H29A,H29B,H29C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C66(H66A,H66B,
 H66C), C69(H69A,H69B,H69C), C26(H26A,H26B,H26C), C71(H71A,H71B,H71C)
;
_olex2_submission_special_instructions 'No special instructions were received'