Open network structures from 2D hydrogen bonded networks: diaminotriazyl tetraoxapentacenes
Maly, Kenneth E.; Buck, William; Dawe, Louise N.; CrystEngComm  (2017) –; doi:10.1039/C7CE01247K

data_7228956
_publ_section_title
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 Open network structures from 2D hydrogen bonded networks: diaminotriazyl
 tetraoxapentacenes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01247K
_journal_year                    2017
_chemical_formula_moiety         'C12 H8 N5 O2, 2(C2 H6 O S), H2 O'
_chemical_formula_sum            'C16 H22 N5 O5 S2'
_chemical_formula_weight         428.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-07-05 deposited with the CCDC.
2017-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.539(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.953(3)
_cell_length_b                   9.0278(18)
_cell_length_c                   20.734(5)
_cell_measurement_reflns_used    9400
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      39.27
_cell_measurement_theta_min      3.18
_cell_volume                     1993.2(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.03
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            126417
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         41.184
_diffrn_reflns_theta_min         2.958
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.6865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0548 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.9177.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.559
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.989
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         12861
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.6008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9784
_reflns_number_total             12861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01247k2.cif
_cod_data_source_block           b16148_0m
_cod_original_cell_volume        1993.3(8)
_cod_database_code               7228956
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O5-H5C \\sim O5-H5D
 with sigma of 0.02
 N4-H4B \\sim N4-H4A \\sim N5-H5A \\sim N5-H5B
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              81837
_olex2_submission_special_instructions 'No special instructions were received'