Studies on sodium polymers based on Di(1H-tetrazol-5-yl) methanone oxime
Guo, Weiming; Zhang, Tonglai; Zhang, Bo; Feng, Yongan; Chen, Sitong; Mi, Zhenhao; RSC Adv.  (2016) –; doi:10.1039/C6RA15591J

data_7226205
_publ_section_title
;
 Studies on sodium polymers based on Di(1H-tetrazol-5-yl) methanone oxime
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA15591J
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C3 H5 N9 Na O3, H4 N O, 0.5(H2 O)'
_chemical_formula_sum            'C3 H10 N10 Na O4.5'
_chemical_formula_weight         281.20
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-12 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.56(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.431(3)
_cell_length_b                   3.5670(7)
_cell_length_c                   22.642(8)
_cell_measurement_reflns_used    3330
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      1.9343
_cell_volume                     1084.0(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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
;
????
;
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 44.8067
              2theta: -20.1860
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.8067
              2theta: -20.1860
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0243
_diffrn_orient_matrix_UB_12      -0.0253
_diffrn_orient_matrix_UB_13      -0.0630
_diffrn_orient_matrix_UB_21      0.0075
_diffrn_orient_matrix_UB_22      0.2610
_diffrn_orient_matrix_UB_23      -0.1020
_diffrn_orient_matrix_UB_31      0.0474
_diffrn_orient_matrix_UB_32      -0.0001
_diffrn_orient_matrix_UB_33      0.0032
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7962
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           90.0000
_diffrn_source_power             4.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.6(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         2480
_refine_ls_number_restraints     392
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+1.0775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1903
_reflns_number_gt                2232
_reflns_number_total             2480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra15591j1.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 H20 N20 Na2 O9'
_cod_original_formula_weight         562.40
_cod_original_formula_moiety         '2(C3 H5 N9 Na O3), 2(H4 N O), H2 O'
_cod_original_formula_units_Z            2
_cod_database_code               7226205
_diffrn_number_total             2881
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.01
3.a Riding coordinates:
 O6(H6A,H6B), N13(H13), O7(H7A,H7B), O3(H3A,H3B), O4(H4A,H4B), N3(H3), O1(H1),
 N21(H21A,H21B,H21C), O2(H2), N22(H22A,H22B,H22C), O5(H5A,H5B)
;
_olex2_submission_special_instructions 'No special instructions were received'