Correlation between Solid-State and Solution Conformational Ratios in a Series of N-(o-Tolyl)Succinimide Molecular Rotors
Li, Ping; Hwang, Jungwun; Maier, Josef M.; Zhao, Chen; Kaborda, Darya V.; Smith, Mark D.; Pellechia, Perry J.; Shimizu, Ken D.; Crystal Growth & Design 15 (2015) 3561–; doi:10.1021/acs.cgd.5b00906

data_4516406
_publ_section_title
;
 Correlation between Solid-State and Solution Conformational Ratios in a
 Series of N-(o-Tolyl)Succinimide Molecular Rotors
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3561
_journal_paper_doi               10.1021/acs.cgd.5b00906
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C30 H23 N O3, 0.5(C7 H8)'
_chemical_formula_sum            'C33.5 H27 N O3'
_chemical_formula_weight         491.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                115.035(2)
_cell_angle_beta                 98.760(2)
_cell_angle_gamma                94.132(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3368(10)
_cell_length_b                   11.1632(11)
_cell_length_c                   12.0626(11)
_cell_measurement_reflns_used    9510
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.498
_cell_measurement_theta_min      2.478
_cell_volume                     1231.9(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14889
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         1.903
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0605P)^2^+0.5788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3521
_reflns_number_total             4240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00906_si_002.cif
_cod_data_source_block           21(lpc79m)
_cod_original_formula_sum        'C33.50 H27 N O3'
_cod_database_code               4516406
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C24A \\sim N1-C24B
 with sigma of 0.015
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C24B)
4. Same fragment restrains
{C24A, C25A, C26A, C27A, C28A, C29A, C30A}
as
{C24B, C25B, C26B, C27B, C28B, C29B, C30B}
5. Others
 Sof(C24B)=Sof(C25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=
 Sof(H28B)=Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=
 Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Fixed Sof: C31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
 C20(H20), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C26A(H26A),
 C27A(H27A), C28A(H28A), C29A(H29A), C26B(H26B), C27B(H27B), C28B(H28B),
 C29B(H29B)
6.c Fitted hexagon refined as free rotating group:
 C31(C32,C33,C34,C35,C36)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C30A(H30A,H30B,
 H30C), C30B(H30D,H30E,H30F)
;
_shelx_res_checksum              7749
_shelx_hkl_checksum              77440
_olex2_submission_special_instructions 'No special instructions were received'