1,2-Bis(4-(1,3-dioxolan-2-yl)phenyl)diazene Oxide
Spesivaya, Ekaterina S.; Lupanova, Ida A.; Konshina, Dzhamilya N.; Konshin, Valery V.; Molbank 2021 (2021) M1224–; doi:10.3390/M1224

data_1563958
_publ_section_title
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 1,2-Bis(4-(1,3-dioxolan-2-yl)phenyl)diazene Oxide
;
_journal_issue                   2
_journal_name_full               Molbank
_journal_page_first              M1224
_journal_paper_doi               10.3390/M1224
_journal_volume                  2021
_journal_year                    2021
_chemical_formula_moiety         'C18 H18 N2 O5'
_chemical_formula_sum            'C18 H18 N2 O5'
_chemical_formula_weight         342.34
_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
_audit_creation_date             2021-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.627(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.5333(7)
_cell_length_b                   21.946(4)
_cell_length_c                   15.968(3)
_cell_measurement_reflns_used    2641
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.73
_cell_volume                     1581.0(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17093
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.619
_diffrn_reflns_theta_min         1.582
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1513 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.8011.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4876
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0607P)^2^+0.8589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3049
_reflns_number_total             4876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s6.cif
_cod_data_source_block           1
_cod_original_cell_volume        1581.0(4)
_cod_database_code               1563958
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.996
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(H9B)=Sof(H6B)=Sof(N2')=Sof(N1')=1-FVAR(1)
 Sof(N1)=Sof(N2)=Sof(H9A)=Sof(H6A)=FVAR(1)
 Sof(C7')=Sof(C8')=Sof(H8')=1-FVAR(2)
 Sof(C7)=Sof(C8)=Sof(H8)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C3(H3A,H3B), C2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C5(H5), C11(H11), C9(H9A), C9(H9B), C15(H15), C6(H6A),
 C6(H6B), C8(H8), C8'(H8')
;
_shelx_res_checksum              99053
_shelx_hkl_checksum              84440
_olex2_submission_special_instructions 'No special instructions were received'