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_4133783
_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 N2 Sc, C18 H36 K N2 O6, 2(C4 H8 O)'
_chemical_formula_sum            'C61 H100 K N4 O8 Sc'
_chemical_formula_weight         1101.50
_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   geom
_atom_sites_solution_primary     direct
_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                 93.986(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1534(3)
_cell_length_b                   21.9933(5)
_cell_length_c                   18.0185(4)
_cell_measurement_reflns_used    33798
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.5840
_cell_measurement_theta_min      3.6430
_cell_volume                     6385.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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     30.00  74.00   0.50    3.67    --   -3.30  38.00 120.00   88
  2  \w    -26.00  28.00   0.50    3.67    --   -3.30 -82.00 -60.00  108
  3  \w     -7.00  31.00   0.50    3.67    --   -3.30 -82.00-180.00   76
  4  \w    -68.00  20.00   0.50    3.67    --   -3.30 -38.00  90.00  176
  5  \w     -6.00  20.00   0.50    3.67    --   -3.30  38.00 120.00   52
  6  \w    -92.00 -46.00   0.50    3.67    --   -3.30 -19.00   0.00   92
  7  \w    -47.00  33.00   0.50    3.67    --    3.60 -77.00 -30.00  160
  8  \w    -23.00  35.00   0.50    3.67    --    3.60 -82.00  60.00  116
  9  \w    -13.00  36.00   0.50    3.67    --    3.60 -82.00  90.00   98
 10  \w    -49.00  24.00   0.50    3.67    --    3.60 -38.00-180.00  146
;
_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      -0.0124223000
_diffrn_orient_matrix_UB_12      -0.0101894000
_diffrn_orient_matrix_UB_13      0.0348903000
_diffrn_orient_matrix_UB_21      0.0041295000
_diffrn_orient_matrix_UB_22      -0.0305899000
_diffrn_orient_matrix_UB_23      -0.0116268000
_diffrn_orient_matrix_UB_31      0.0420235000
_diffrn_orient_matrix_UB_32      0.0000094000
_diffrn_orient_matrix_UB_33      0.0143387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            115203
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.392
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         12521
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0710P)^2^+3.2199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10902
_reflns_number_total             12521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11631_si_002.cif
_cod_data_source_block           2a-crypt_(THF)2
_cod_depositor_comments
'Adding full bibliography for 4133782--4133791.cif.'
_cod_database_code               4133783
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sc C H N O K'
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 99.72
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C55-C54
 1.54 with sigma of 0.01
3. Others
 Sof(O7B)=Sof(H58C)=Sof(H58D)=Sof(H61C)=Sof(H61D)=1-FVAR(1)
 Sof(O7A)=Sof(H58A)=Sof(H58B)=Sof(H61A)=Sof(H61B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23)
4.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C58(H58A,H58B), C58(H58C,H58D),
 C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C61(H61C,H61D), C54(H54A,H54B),
  C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_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 2.125
_oxdiff_exptl_absorpt_empirical_full_min 0.716