Molecular Coplanarity and Self-Assembly Promoted by Intramolecular Hydrogen Bonds.
Zhu, Congzhi; Mu, Anthony U.; Lin, Yen-Hao; Guo, Zi-Hao; Yuan, Tianyu; Wheeler, Steven E.; Fang, Lei; Organic letters 18 (2016) 6332–6335; doi:10.1021/acs.orglett.6b03225

data_1555962
_publ_section_title
;
 Molecular Coplanarity and Self-Assembly Promoted by Intramolecular
 Hydrogen Bonds.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6332
_journal_page_last               6335
_journal_paper_doi               10.1021/acs.orglett.6b03225
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C2 H2 Cl4, C55 H50 N2 O7'
_chemical_formula_sum            'C57 H52 Cl4 N2 O7'
_chemical_formula_weight         1018.80
_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             2016-06-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.032(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5586(7)
_cell_length_b                   37.6596(19)
_cell_length_c                   12.2407(7)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      57.895
_cell_measurement_theta_min      2.346
_cell_volume                     5005.9(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      100.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26450
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        50.000
_diffrn_reflns_theta_max         50.000
_diffrn_reflns_theta_min         2.346
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.604
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.5691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1257 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.7574.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         5102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0875
_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^)+(0.0302P)^2^+24.9058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3508
_reflns_number_total             5102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03225_si_002.cif
_cod_data_source_block           c8hmodel
_cod_database_code               1555962
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.493
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S)
2.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B), C49(H49A,H49B),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C13(H13), C14(H14), C15(H15), C20(H20), C21(H21), C22(H22),
 C23(H23), C27(H27), C28(H28), C29(H29), C36(H36), C37(H37), C38(H38), C39(H39)
2.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              99676
_shelx_hkl_checksum              45448
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'