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_4133788
_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         'C35 H48 N4 O Sc, C18 H36 K N2 O6'
_chemical_formula_sum            'C53 H84 K N6 O7 Sc'
_chemical_formula_weight         1001.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 103.475(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7441(4)
_cell_length_b                   25.3512(7)
_cell_length_c                   21.2161(6)
_cell_measurement_reflns_used    24668
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      28.8010
_cell_measurement_theta_min      2.5290
_cell_volume                     5619.7(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -44.00  82.00   0.50    4.60    --   -5.70  23.00 -96.00  252
  2  \w    -33.00  17.00   0.50    4.60    --   -5.70 -82.00  60.00  100
  3  \w    -89.00  24.00   0.50    4.60    --   -5.70 -37.00-120.00  226
  4  \w    -46.00  -2.00   0.50    4.60    --   -5.70 -77.00-180.00   88
  5  \w     -4.00  30.00   0.50    4.60    --   -5.70 -82.00 120.00   68
  6  \w      7.00  95.00   0.50    4.60    --    6.00  57.00 150.00  176
  7  \w     -3.00  69.00   0.50    4.60    --    6.00  19.00  60.00  144
  8  \w    -45.00  34.00   0.50    4.60    --    6.00 -57.00  30.00  158
;
_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      -0.0304664000
_diffrn_orient_matrix_UB_12      -0.0085025000
_diffrn_orient_matrix_UB_13      -0.0185624000
_diffrn_orient_matrix_UB_21      0.0126358000
_diffrn_orient_matrix_UB_22      -0.0001088000
_diffrn_orient_matrix_UB_23      -0.0277787000
_diffrn_orient_matrix_UB_31      0.0096777000
_diffrn_orient_matrix_UB_32      -0.0266632000
_diffrn_orient_matrix_UB_33      0.0060028000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102744
_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         26.022
_diffrn_reflns_theta_min         1.974
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92802
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         11061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+2.9853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9754
_reflns_number_total             11061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11631_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4133782--4133791.cif.'
_cod_database_code               4133788
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'CH N O P S'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H31A,H31B,H31C} of C31, {H33A,H33B,H33C} of C33, {H22A,
  H22B,H22C} of C22, {H16A,H16B,H16C} of C16, {H25A,H25B,H25C} of C25, {H24A,
  H24B,H24C} of C24, {H35A,H35B,H35C} of C35, All C(H,H) groups
 At 1.5 times of:
  {H34A,H34B,H34C} of C34, {H17A,H17B,H17C} of C17, {H32A,H32B,H32C} of C32
2.a Riding coordinates:
 C4(H4), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16A,H16B,
 H16C), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B,H22C),
 C23(H23), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C),
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
2.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C49(H49A,H49B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_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 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.770