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_4516410
_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         'C41 H26 N2 O3'
_chemical_formula_sum            'C41 H26 N2 O3'
_chemical_formula_weight         594.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.823(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.161(2)
_cell_length_b                   17.4083(16)
_cell_length_c                   16.5300(15)
_cell_measurement_reflns_used    8949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.468
_cell_measurement_theta_min      2.320
_cell_volume                     5652.9(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0587
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            90080
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.509
_diffrn_reflns_theta_min         1.563
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.873109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0772 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.8731.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         11675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0460P)^2^+5.9931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                9682
_reflns_number_total             11675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00906_si_002.cif
_cod_data_source_block           30(jmm234)
_cod_original_cell_volume        5653.0(9)
_cod_database_code               4516410
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.952
_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.a Ternary CH refined with riding coordinates:
 C3A(H3A), C6A(H6A), C3B(H3B), C6B(H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C11A(H11A), C12A(H12A), C13A(H13A), C15A(H15A), C16A(H16A), C18A(H18A),
 C19A(H19A), C20A(H20A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A),
 C29A(H29A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A),
 C38A(H38A), C39A(H39A), C40A(H40A), C11B(H11B), C12B(H12B), C13B(H13B),
 C15B(H15B), C16B(H16B), C18B(H18B), C19B(H19B), C20B(H20B), C25B(H25B),
 C26B(H26B), C27B(H27B), C28B(H28B), C29B(H29B), C31B(H31B), C32B(H32B),
 C33B(H33B), C34B(H34B), C35B(H35B), C38B(H38B), C39B(H39B), C40B(H40B)
2.c Idealised Me refined as rotating group:
 C41A(H41A,H41B,H41C), C41B(H41D,H41E,H41F)
;
_shelx_res_checksum              16388
_shelx_hkl_checksum              56276
_olex2_submission_special_instructions 'No special instructions were received'