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_4516399
_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         'C31 H23 N O5, C2 H3 N'
_chemical_formula_sum            'C33 H26 N2 O5'
_chemical_formula_weight         530.56
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                87.907(2)
_cell_angle_beta                 86.025(2)
_cell_angle_gamma                63.842(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6779(8)
_cell_length_b                   9.7233(8)
_cell_length_c                   15.3703(12)
_cell_measurement_reflns_used    6455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.360
_cell_measurement_theta_min      2.334
_cell_volume                     1295.08(18)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0553
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16142
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.328
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4534
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0428P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                3276
_reflns_number_total             4534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00906_si_002.cif
_cod_data_source_block           10(lpc195am)
_cod_database_code               4516399
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.978
_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. Shared sites
{C24A, C24B}
{C25A, C29B}
{C26A, C28B}
{C27A, C27B}
{C28A, C26B}
{C29A, C25B}
3. Restrained distances
 C25A-C30A \\sim C25B-C30B
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C24B)
Uanis(C25A) = Uanis(C29B)
Uanis(C26A) = Uanis(C28B)
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C26B)
Uanis(C29A) = Uanis(C25B)
5. Others
 Sof(C24B)=Sof(C25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=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(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
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), C26A(H26A), C28A(H28A), C29A(H29A), C26B(H26B), C28B(H28B),
 C29B(H29B)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              45113
_shelx_hkl_checksum              684
_olex2_submission_special_instructions 'No special instructions were received'