Tetraphenylethylene tetracylhydrazine macrocycle with capability for discrimination of n-propanol from i-propanol and highly sensitive/selective detection of nitrobenzene
Xie, Wen-Zhao; Zhang, Hong-Chao; Zheng, Yan-Song; J. Mater. Chem. C 5 (2017) 10462–; doi:10.1039/C7TC02525D

data_7236841
_publ_section_title
;
 Tetraphenylethylene tetracylhydrazine macrocycle with capability for
 discrimination of n-propanol from i-propanol and highly
 sensitive/selective detection of nitrobenzene
;
_journal_issue                   40
_journal_name_full               'J. Mater. Chem. C'
_journal_page_first              10462
_journal_paper_doi               10.1039/C7TC02525D
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C50 H48 N2 O4, C2 H6 O'
_chemical_formula_sum            'C52 H54 N2 O5'
_chemical_formula_weight         786.97
_chemical_melting_point          282.5(5)
_chemical_name_systematic        'TPEtetracylhydrazine macrocycle'
_chemical_properties_physical    ', Efflorescent'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-06-05 deposited with the CCDC.
2017-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.749(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.906(10)
_cell_length_b                   9.493(2)
_cell_length_c                   27.486(7)
_cell_measurement_reflns_used    4630
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.21
_cell_volume                     9901(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            40424
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.073
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0769 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.7758.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform and ethanol'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         11291
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1651P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6075
_reflns_number_total             11291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7tc02525d2.cif
_cod_data_source_block           mo_dm15646_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '282-283' was changed to
'282.5(5)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7236841
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.974
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C46(H46A,
 H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12),
 C13(H13), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C30(H30), C31(H31), C33(H33), C34(H34), C41(H41), C42(H42),
 C44(H44), C45(H45)
3.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              35759
_shelx_hkl_checksum              57078
_olex2_submission_special_instructions 'No special instructions were received'