Well-Defined Scandacyclopropenes: Synthesis, Structure, and Reactivity.
Lv, Ze-Jie; Huang, Zhe; Shen, Jinghang; Zhang, Wen-Xiong; Xi, Zhenfeng; Journal of the American Chemical Society 141 (2019) 20547–20555; doi:10.1021/jacs.9b11631

data_4133785
_publ_section_title
;
 Well-Defined Scandacyclopropenes: Synthesis, Structure, and Reactivity.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20547
_journal_page_last               20555
_journal_paper_doi               10.1021/jacs.9b11631
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C41 H56 K N2 O Sc'
_chemical_formula_sum            'C41 H56 K N2 O Sc'
_chemical_formula_weight         676.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.273(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.869(3)
_cell_length_b                   8.6245(9)
_cell_length_c                   20.838(3)
_cell_measurement_reflns_used    3880
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.2090
_cell_measurement_theta_min      3.9000
_cell_volume                     3924.6(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -16.00  22.00   0.50   22.00    --    1.90  57.00-150.00   76
  2  \w     53.00  91.00   0.50   22.00    --    1.90  57.00-150.00   76
  3  \w    -67.00  19.00   0.50   22.00    --    1.90 -38.00-120.00  172
  4  \w    -26.00  34.00   0.50   22.00    --    1.90 -82.00 150.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0319273000
_diffrn_orient_matrix_UB_12      -0.0132701000
_diffrn_orient_matrix_UB_13      0.0074305000
_diffrn_orient_matrix_UB_21      0.0054244000
_diffrn_orient_matrix_UB_22      0.0488863000
_diffrn_orient_matrix_UB_23      0.0283430000
_diffrn_orient_matrix_UB_31      -0.0023323000
_diffrn_orient_matrix_UB_32      -0.0648031000
_diffrn_orient_matrix_UB_33      0.0202182000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28658
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.572
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7630
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0457P)^2^+5.8501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6251
_reflns_number_total             7630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11631_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4133782--4133791.cif.'
_cod_original_cell_volume        3924.7(10)
_cod_database_code               4133785
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sc1 C1 H1 K1'
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.938
_reflns_odcompleteness_completeness 97.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Rigid bond restraints
 C40, C41
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C41, C42
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Ternary CH refined with riding coordinates:
 C36(H36), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C34(H34A,H34B), C33(H33A,H33B), C39(H39A,H39B), C42(H42A,
 H42B), C40(H40A,H40B), C41(H41A,H41B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C4(H4), C14(H14), C13(H13), C15(H15), C8(H8), C5(H5),
 C6(H6), C7(H7)
3.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C), C38(H38A,
 H38B,H38C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.481