Synthesis and Structure of 3,3-Dimethylindoline Squaraine Rotaxanes.
Jarvis, Tia S.; Collins, Carleton G.; Dempsey, Janel M.; Oliver, Allen G.; Smith, Bradley D.; The Journal of organic chemistry 82 (2017) 5819–5825; doi:10.1021/acs.joc.7b00655

data_4032554
_publ_section_title
;
 Synthesis and Structure of 3,3-Dimethylindoline Squaraine Rotaxanes.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5819
_journal_page_last               5825
_journal_paper_doi               10.1021/acs.joc.7b00655
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C56 H52 N4 O4, C28 H28 N2 O4'
_chemical_formula_sum            'C84 H80 N6 O8'
_chemical_formula_weight         1301.54
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 112.420(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9997(5)
_cell_length_b                   25.0507(12)
_cell_length_c                   13.0048(6)
_cell_measurement_reflns_used    5782
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.94
_cell_measurement_theta_min      3.53
_cell_volume                     3312.6(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44055
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.229
_diffrn_reflns_theta_min         3.529
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       plate
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6502
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+2.8970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2227
_refine_ls_wR_factor_ref         0.2358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5314
_reflns_number_total             6502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00655_si_002.cif
_cod_data_source_block           nd1604
_cod_database_code               4032554
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.985
_diffrn_source_monochromator     'MONTEL Multi-layer'
_shelx_res_checksum              6256
_shelx_hkl_checksum              75459