Alkali and alkaline earth metal salts of tetrazolone: structurally interesting and excellently thermostable
He, Piao; Wu, Le; Wu, Jin-Ting; Yin, Xin; Gozin, Michael; Zhang, Jian-Guo; Dalton Trans.  (2017) –; doi:10.1039/C7DT01179B

data_7043371
_publ_section_title
;
 Alkali and alkaline earth metal salts of tetrazolone: structurally
 interesting and excellently thermostable
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01179B
_journal_year                    2017
_chemical_formula_moiety
'C4 H24 Ca2 N16 O14, 0.5(C2 H4 N8 O2), 0.5(H4 O2)'
_chemical_formula_sum            'C5 H28 Ca2 N20 O16'
_chemical_formula_weight         704.63
_chemical_name_systematic        'Calcium 5-oxotetrazolate pentahydrate '
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-25 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9853(10)
_cell_length_b                   24.4542(15)
_cell_length_c                   6.7717(3)
_cell_measurement_reflns_used    2606
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.433
_cell_measurement_theta_min      2.843
_cell_volume                     2481.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1171
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         2.845
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.9086
_exptl_absorpt_correction_T_min  0.8026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.761
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1171
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.1290
_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^)+(0.1272P)^2^+64.1440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2995
_refine_ls_wR_factor_ref         0.3075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1000
_reflns_number_total             1171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01179b2.cif
_cod_data_source_block           140725g
_cod_database_code               7043371
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.803
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.889(9)
 0.111(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 N12-C3 = N9-C3
 1.33 with sigma of 0.02
 N12-N11 = N9-N10
 1.33 with sigma of 0.02
4. 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
5. Others
 Fixed Sof: N9(0.25) H9(0.25) N10(0.25) N11(0.25) N12(0.25) H12(0.25) O3(0.25)
 O7(0.25) H7A(0.25) H7B(0.25) C3(0.25)
6.a Fixed occupancy and ADP/Uiso:
 H4
6.b Riding coordinates:
 N9(H9), N12(H12), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'