Lithium Dicyclohexylamide in Transition-Metal-Free Fischer-Tropsch Chemistry.
Xu, Maotong; Qu, Zheng-Wang; Grimme, Stefan; Stephan, Douglas W.; Journal of the American Chemical Society 143 (2021) 634–638; doi:10.1021/jacs.0c11482

data_4135570
_publ_section_title
;
 Lithium Dicyclohexylamide in Transition-Metal-Free Fischer-Tropsch
 Chemistry.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              634
_journal_page_last               638
_journal_paper_doi               10.1021/jacs.0c11482
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C27 H46 N2 O3'
_chemical_formula_sum            'C30 H20 N2 O2'
_chemical_formula_weight         440.48
_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
_audit_creation_date             2020-12-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                80.371(18)
_cell_angle_beta                 87.27(3)
_cell_angle_gamma                67.96(3)
_cell_formula_units_Z            2
_cell_length_a                   7.918(6)
_cell_length_b                   9.651(6)
_cell_length_c                   17.999(13)
_cell_measurement_reflns_used    319
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.49
_cell_measurement_theta_min      2.74
_cell_volume                     1256.8(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1533
_diffrn_reflns_av_unetI/netI     0.1218
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28036
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        23.549
_diffrn_reflns_theta_max         23.549
_diffrn_reflns_theta_min         2.405
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.6792
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1469 before and 0.1128 after correction.
The Ratio of minimum to maximum transmission is 0.8883.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       SHARD
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0872P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2378
_reflns_number_total             3695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Cy2NC(O)CH(OH)NCy2.cif
_cod_data_source_block           final_a
_cod_original_cell_volume        1256.6(15)
_cod_database_code               4135570
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.996
_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) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C11(H11), C2(H2A), C41(H41), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C42(H42A,H42B), C16(H16A,H16B), C46(H46A,H46B), C33(H33A,
 H33B), C12(H12A,H12B), C13(H13A,H13B), C26(H26A,H26B), C36(H36A,H36B),
 C32(H32A,H32B), C43(H43A,H43B), C45(H45A,H45B), C25(H25A,H25B), C34(H34A,H34B),
  C35(H35A,H35B), C44(H44A,H44B), C14(H14A,H14B), C23(H23A,H23B), C15(H15A,
 H15B), C24(H24A,H24B)
;
_shelx_res_checksum              78287
_shelx_hkl_checksum              39644
_olex2_submission_special_instructions 'No special instructions were received'