[Na4(N5)4(H2O)2]·H2O·2MeOH: a honeycomb-like sodium pentazolate framework with helical chains
Xu, Yuangang; Xu, Ze; Zhang, Xiaopeng; Hou, Tianyang; Lu, Ming; CrystEngComm  (2022) –; doi:10.1039/D2CE00713D

data_7245132
_publ_section_title
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 [Na4(N5)4(H2O)2]&#x00B7;H2O&#x00B7;2MeOH: a honeycomb-like sodium
 pentazolate framework with helical chains
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00713D
_journal_year                    2022
_chemical_formula_moiety         'H2 N10 Na2 O, 0.5(H2 O), C H4 O'
_chemical_formula_sum            'C H7 N10 Na2 O2.5'
_chemical_formula_weight         245.15
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2019-01-30 deposited with the CCDC.	2022-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.6556(6)
_cell_length_b                   9.6556(6)
_cell_length_c                   18.7426(9)
_cell_measurement_reflns_used    9535
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.462
_cell_measurement_theta_min      2.670
_cell_volume                     1513.28(15)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.977
_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  0.0813
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12964
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         2.667
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.6403
_exptl_absorpt_correction_T_min  0.5493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1717 before and 0.1205 after correction. The Ratio of minimum to maximum transmission is 0.8579. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       needle
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 793 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2285
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0970P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                2143
_reflns_number_total             2285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00713d2.cif
_cod_data_source_block           22019102331_0m
_cod_original_cell_volume        1513.3(2)
_cod_original_formula_sum        'C H7 N10 Na2 O2.50'
_cod_database_code               7245132
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.643(4)
 0.357(4)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, {H3A,H3B} of O3, All O(H) groups
 At 1.2 times of:
  {H1A,H1B} of O1
3. Restrained distances
 O1-H1B = O1-H1A
 0.86 with sigma of 0.005
 H2-H3B
 2.1 with sigma of 0.005
 H1B-H1A
 1.39 with sigma of 0.005
4. Others
 Fixed Sof: H3A(0.5) H3B(0.5)
5.a Riding coordinates:
 O1(H1A,H1B)
5.b Free rotating group:
 O3(H3A,H3B)
5.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
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_shelx_res_checksum              44255
_olex2_submission_special_instructions 'No special instructions were received'