Selectivity in Olefin-Intervened Macrocyclic Ring-Closing Metathesis
Liu, Ruzhang; Ge, Hua; Chen, Kuanwei; Xue, Huaiguo; ACS Catalysis 8 (2018) 5574–; doi:10.1021/acscatal.8b01084

data_4515649
_publ_section_title
;
 Selectivity in Olefin-Intervened Macrocyclic Ring-Closing Metathesis
;
_journal_issue                   6
_journal_name_full               'ACS Catalysis'
_journal_page_first              5574
_journal_paper_doi               10.1021/acscatal.8b01084
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C30 H42 N2 O4 S2'
_chemical_formula_sum            'C30 H42 N2 O4 S2'
_chemical_formula_weight         558.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5361)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.802(5)
_cell_length_b                   8.4124(14)
_cell_length_c                   10.9145(15)
_cell_measurement_reflns_used    3717
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2.50
_cell_measurement_theta_min      27.01
_cell_volume                     3011.8(8)
_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_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_unetI/netI     0.1336
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21429
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         1.242
_exptl_absorpt_coefficient_mu    0.213
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 783 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.50(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4960
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.2129
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1170P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2245
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                2357
_reflns_number_total             4960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b01084_si_002.cif
_cod_data_source_block           ZZ-3
_cod_database_code               4515649
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.943
_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. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C14) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
3.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C13(H13a,H13b), C14(H14a,H14b),
 C15(H15a,H15b), C16(H16a,H16b), C17(H17a,H17b), C18(H18a,H18b), C21(H21a,H21b),
  C22(H22a,H22b), C23(H23a,H23b)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C11(H11), C12(H12), C19(H19), C20(H20),
 C25(H25), C26(H26), C29(H29), C30(H30)
3.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C28(H28a,H28b,H28c)
;
_shelx_res_checksum              47940
_shelx_hkl_checksum              66944
_olex2_submission_special_instructions 'No special instructions were received'