Synthesis, structure and catalytic activity of organozinc complexes derived from chiral sulfonylamidoazetidines
Zhao, Hongyan; Zhang, Shaohui; Fang, Xiaojun; Chen, Liang; Ren, Wenshan; Inorganica Chimica Acta 511 (2020) 119767–; doi:10.1016/j.ica.2020.119767

data_1564151
_publ_section_title
;
 Synthesis, structure and catalytic activity of organozinc complexes
 derived from chiral sulfonylamidoazetidines
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119767
_journal_paper_doi               10.1016/j.ica.2020.119767
_journal_volume                  511
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C52 H60 N4 O4 S2 Zn2'
_chemical_formula_sum            'C52 H60 N4 O4 S2 Zn2'
_chemical_formula_weight         999.90
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.5916(2)
_cell_length_b                   11.5916(2)
_cell_length_c                   34.5612(5)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    290.73(10)
_cell_measurement_theta_max      72.6890
_cell_measurement_theta_min      4.3890
_cell_volume                     4021.67(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.73(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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    -91.00  -3.00   1.00    2.94    --  -37.03 126.00 -90.00   88
  2  \w   -104.00 -20.00   1.00    2.94    --  -37.03 -57.00  30.00   84
  3  \w      1.00  76.00   1.00    2.94    --   37.03 -99.00  30.00   75
  4  \w     24.00  91.00   1.00    2.94    --   37.03-126.00 -30.00   67
  5  \w    -30.00  54.00   1.00    2.94    --   37.03 -57.00 -90.00   84
  6  \w     24.00  91.00   1.00    2.94    --   37.03-126.00-150.00   67
  7  \w     41.00 109.00   1.00   15.00    --  110.47 -95.00-180.00   68
  8  \w     41.00 109.00   1.00   15.00    --  110.47 -95.00   0.00   68
  9  \w     42.00 128.00   1.00   15.00    --  110.47 -45.00   0.00   86
 10  \w     41.00 116.00   1.00   15.00    --  110.47-112.00 -30.00   75
 11  \w     40.00 149.00   1.00   15.00    --  110.47 -15.00   0.00  109
 12  \w   -105.00 -10.00   1.00    2.94    --  -37.03 -77.00-180.00   95
 13  \w    -66.00  34.00   1.00    2.94    --  -37.03  19.00-150.00  100
 14  \w   -106.00 -66.00   1.00    2.94    --  -37.03 -38.00  60.00   40
 15  \w   -104.00 -20.00   1.00    2.94    --  -37.03 -57.00 -90.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1389424000
_diffrn_orient_matrix_UB_12      -0.1072190000
_diffrn_orient_matrix_UB_13      0.0141380000
_diffrn_orient_matrix_UB_21      -0.0397804000
_diffrn_orient_matrix_UB_22      0.1074987000
_diffrn_orient_matrix_UB_23      0.0052850000
_diffrn_orient_matrix_UB_31      -0.0518043000
_diffrn_orient_matrix_UB_32      -0.0225748000
_diffrn_orient_matrix_UB_33      -0.0419204000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            19974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.040
_diffrn_reflns_theta_min         3.837
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.174
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (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    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1590 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0729P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                4662
_reflns_number_total             5265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-511-119767.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        4021.67(15)
_cod_database_code               1564151
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.670
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C4(H4), C19(H19), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C6(H6), C18(H18), C16(H16), C22(H22), C7(H7), C15(H15), C11(H11),
 C10(H10), C14(H14), C23(H23), C24(H24), C25(H25), C26(H26)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C20(H20A,H20B,H20C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              65616
_shelx_hkl_checksum              24185
_shelx_fab_checksum              65447