A Carbon-free Inorganic-metal Complex Consisting of All-nitrogen Pentazole Anion, Zn(II) Cation and H2O
Xu, Yuangang; Wang, Pengcheng; Lin, Qiuhan; Lu, Ming; Dalton Trans.  (2017) –; doi:10.1039/C7DT03231E

data_7044354
_publ_section_title
;
 A Carbon-free Inorganic-metal Complex Consisting of All-nitrogen
 Pentazole Anion, Zn(II) Cation and H2O
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03231E
_journal_year                    2017
_chemical_formula_moiety         'H8 N10 O4 Zn, 2(H4 O2)'
_chemical_formula_sum            'H16 N10 O8 Zn'
_chemical_formula_weight         349.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-20 deposited with the CCDC.
2017-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.293(4)
_cell_length_b                   17.319(6)
_cell_length_c                   6.536(2)
_cell_measurement_reflns_used    2611
_cell_measurement_temperature    205
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.35
_cell_volume                     1391.5(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      205
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.987
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2971
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.257
_diffrn_reflns_theta_min         3.315
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1033 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.6603. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.045(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0473P)^2^+1.1970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                452
_reflns_number_total             453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03231e2.cif
_cod_data_source_block           mo_nlg-x-70_0ma
_cod_original_cell_volume        1391.5(9)
_cod_database_code               7044354
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H1B(0.5) H1A(0.5)
3.a Free rotating group:
 O2(H2A,H2B)
3.b Rotating group:
 O1(H1B,H1A)
;
_olex2_submission_special_instructions 'No special instructions were received'