Advancing nonlinear optics: discovery and characterization of new non-centrosymmetric phenazine-based halides.
Cui, Yibo; Cao, Jindong; Lin, Jiawei; Li, Chunxiao; Yao, Jiyong; Liu, Kunjie; Hou, An; Guo, Zhongnan; Zhao, Jing; Liu, Quanlin; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10235–10243; doi:10.1039/d4dt01096e

data_7716227
_publ_section_title
;
 Advancing nonlinear optics: discovery and characterization of new
 non-centrosymmetric phenazine-based halides.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10235
_journal_page_last               10243
_journal_paper_doi               10.1039/d4dt01096e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Cl4 Sb, C12 H9 N2'
_chemical_formula_sum            'C12 H9 Cl4 N2 Sb'
_chemical_formula_weight         444.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-20 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.189(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.72281(15)
_cell_length_b                   15.2642(5)
_cell_length_c                   17.5395(5)
_cell_measurement_reflns_used    8357
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9300
_cell_measurement_theta_min      3.7490
_cell_volume                     1520.10(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17233
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.440
_diffrn_reflns_theta_min         3.512
_exptl_absorpt_coefficient_mu    2.504
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(8)
_refine_ls_extinction_coef       0.0371(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0285P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.778
_reflns_number_gt                5757
_reflns_number_total             7017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01096e2.cif
_cod_data_source_block           p21
_cod_depositor_comments
'Adding full bibliography for 7716226--7716228.cif.'
_cod_original_cell_volume        1520.11(7)
_cod_database_code               7716227
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.67(8)
 0.33(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Rigid bond restraints
 C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3
 with sigma for 1-2 distances of 1.7 and sigma for 1-3 distances of 1.7
4. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C13) = Uanis(C14)
5.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1), C7(H7), C15(H15), C14(H14), C9(H9), C6(H6), C18(H18),
 C12(H12), C3(H3), C2(H2), C1(H1A), C21(H21), C24(H24), C19(H19), C13(H13),
 C8(H8), C20(H20)
;
_shelx_res_checksum              42096
_shelx_hkl_checksum              31649
_olex2_submission_special_instructions 'No special instructions were received'