Phenanthroimidazole derivatives as a chemosensor for picric acid: a first realistic approach
Ahmed, Ruby; Ali, Abid; Ahmad, Musheer; Alsalme, Ali; Khan, Rais Ahmad; Ali, Farman; New Journal of Chemistry 44 (2020) 20092–20100; doi:10.1039/D0NJ03422C

data_7060228
_publ_section_title
;
 Phenanthroimidazole derivatives as a chemosensor for picric acid: a first
 realistic approach
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20092
_journal_page_last               20100
_journal_paper_doi               10.1039/D0NJ03422C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'C2 H6 O S, C6 H2 N3 O7, C31 H19 N2, 1[C2H6SO]'
_chemical_formula_sum            'C41 H33 N5 O9 S2'
_chemical_formula_weight         803.879
_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_Int_Tables_number      14
_audit_creation_date             2020-08-17
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.07.30 svn.rde3f2a17 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.342(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4343(5)
_cell_length_b                   30.238(2)
_cell_length_c                   16.0736(11)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.11
_cell_measurement_theta_min      3.19
_cell_volume                     3575.1(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.9983
_diffrn_reflns_Laue_measured_fraction_max 0.9983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57453
_diffrn_reflns_point_group_measured_fraction_full 0.9983
_diffrn_reflns_point_group_measured_fraction_max 0.9983
_diffrn_reflns_theta_full        25.0498
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.9190.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             1673.842
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.3053
_refine_diff_density_min         -0.3994
_refine_diff_density_rms         0.0638
_refine_ls_d_res_high            0.8393
_refine_ls_d_res_low             7.3556
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     534
_refine_ls_number_reflns         6312
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.0856
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+1.7116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5041
_reflns_number_total             6312
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0nj03422c2.cif
_cod_data_source_block           3octd_0m_a
_cod_original_formula_sum        'C41 H33 N5 O9 S2 '
_cod_database_code               7060228
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-C37 \\sim O6A-C37
 with sigma of 0.04
 O7-N5 \\sim O7A-N5A
 with sigma of 0.02
 O7-C37 \\sim O7A-C37
 with sigma of 0.04
 O6-O7 \\sim O6A-O7A
 with sigma of 0.04
 N5-C37 \\sim N5A-C37
 with sigma of 0.02
 O6-N5 \\sim O6A-N5A
 with sigma of 0.02
 O3-C33 \\sim O3A-C33
 with sigma of 0.04
 O2-O3 \\sim O2A-O3A
 with sigma of 0.04
 O2-N3 \\sim O2A-N3A
 with sigma of 0.02
 O2-C33 \\sim O2A-C33
 with sigma of 0.04
 O3-N3 \\sim O3A-N3A
 with sigma of 0.02
 N3-C33 \\sim N3A-C33
 with sigma of 0.02
3. Restrained planarity
 C33, O2A, O3A, N3A
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(N3A) = Uanis(N3)
5. Rigid body (RIGU) restrains
 O3A, N3A, O2A, O2, N3, O3, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(O6A)=Sof(O7A)=Sof(N5A)=1-FVAR(1)
 Sof(O6)=Sof(O7)=Sof(N5)=FVAR(1)
 Fixed Sof: O2(0.85) O3(0.85) N3(0.85) O2A(0.15) O3A(0.15) N3A(0.15)
7.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C36(H36), N2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10),
 C11(H11), C12(H12), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C27(H27), C28(H28)
7.b Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C39(H39a,H39b,H39c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 180 electrons were 
found in a volume of 492\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[C2H6SO] per Formula
Unit which account for 168 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'