#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:02:19 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258805 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/56/7705692.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7705692
loop_
_publ_author_name
'Westwater, Bradley'
'Lloyd, Hayleigh J.'
'Vitorica-Yrezabal, Inigo J'
'Fong, Angela'
'McMaster, Patrick'
'Sloan, Martin'
'Coaker, Brian M.'
'Pulham, Colin R.'
'Portius, Peter'
_publ_section_title
;
 Synthesis and characterization of the mixed-ligand coordination polymer
 Cu₃Cl(N₄C-NO₂)₂.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14975
_journal_page_last               14984
_journal_paper_doi               10.1039/d0dt03077e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '0.5(C2 H8 N10 Na2 O8), 2(H2 O)'
_chemical_formula_sum            'C H8 N5 Na O6'
_chemical_formula_weight         209.11
_chemical_name_systematic        'Sodium nitrotetrazolate tetrahydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-28 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.282(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7189(10)
_cell_length_b                   3.5053(2)
_cell_length_c                   13.3457(8)
_cell_measurement_reflns_used    6147
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.75
_cell_measurement_theta_min      3.37
_cell_volume                     815.59(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2017)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9009
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.741
_diffrn_reflns_theta_max         66.741
_diffrn_reflns_theta_min         5.073
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1391 before and 0.0946 after correction. The Ratio of minimum to maximum transmission is 0.7007. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         710
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0390
_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/[σ²(Fo²)+(0.0517P)²+1.1521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                673
_reflns_number_total             710
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03077e2.cif
_cod_data_source_block           ch1ppx451v_0m
_cod_depositor_comments
'Adding full bibliography for 7705692--7705693.cif.'
_cod_database_code               7705692
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O3-H3B = O3-H3A
 0.87 with sigma of 0.02
 O4-H4B = O4-H4A
 0.87 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O1(0.5) O2(0.5) N1(0.5) N2(0.5) N3(0.5) N4(0.5) N5(0.5)
5.a Free rotating group:
 O4(H4A)
;
_olex2_exptl_crystal_mounting_method 'Mitigen microloop in fombin oil'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.7500 0.2500 0.5000 0.0116(3) Uani 1 2 d S TU P . .
O1 O 0.8852(5) 0.232(3) 0.5126(7) 0.0168(18) Uani 0.5 1 d . U . A -1
O2 O 0.4564(4) -0.050(2) 0.6510(4) 0.0192(14) Uani 0.5 1 d . U . B -1
O3 O 0.74998(7) 0.7476(3) 0.62075(10) 0.0128(4) Uani 1 1 d D U . . .
H3A H 0.7859(12) 0.800(7) 0.6687(16) 0.024(6) Uiso 1 1 d D . . . .
H3B H 0.7124(16) 0.709(11) 0.652(3) 0.066(11) Uiso 1 1 d D . . . .
N1 N 0.6025(7) 0.217(4) 0.4648(8) 0.0101(15) Uani 0.5 1 d . U . A -1
N2 N 0.56574(16) 0.1652(9) 0.5438(2) 0.0098(6) Uani 0.5 1 d . U . A -1
N3 N 0.49383(16) -0.0633(9) 0.4012(2) 0.0101(6) Uani 0.5 1 d . U . A -1
N4 N 0.5593(4) 0.079(3) 0.3793(7) 0.0123(13) Uani 0.5 1 d . U . A -1
N5 N 0.4426(3) -0.1139(10) 0.5588(4) 0.0106(7) Uani 0.5 1 d . U . B -1
C1 C 0.5000 0.0000 0.5000 0.0085(5) Uani 1 2 d S TU P . .
O4 O 0.63351(7) 0.5186(4) 0.72616(9) 0.0143(4) Uani 1 1 d D U . . .
H4A H 0.6009 0.3750 0.6866 0.021 Uiso 1 1 d DG . . . .
H4B H 0.6055(14) 0.677(7) 0.749(2) 0.034(7) Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Na1 Na1 Na1 180.0 1_545 1_565 ?
O1 Na1 Na1 88.5(3) . 1_545 ?
O1 Na1 Na1 91.5(3) . 1_565 ?
O1 Na1 O3 93.1(3) . 1_545 ?
O1 Na1 O3 86.9(3) . 7_666 ?
O1 Na1 O3 95.4(2) . . ?
O1 Na1 O3 84.6(2) . 7_656 ?
O1 Na1 N1 172.4(4) . . ?
O3 Na1 Na1 42.74(3) . 1_565 ?
O3 Na1 Na1 137.26(3) . 1_545 ?
O3 Na1 Na1 137.26(3) 7_656 1_565 ?
O3 Na1 Na1 137.54(3) 7_666 1_545 ?
O3 Na1 Na1 137.54(3) 1_545 1_565 ?
O3 Na1 Na1 42.46(3) 7_666 1_565 ?
O3 Na1 Na1 42.74(3) 7_656 1_545 ?
O3 Na1 Na1 42.46(3) 1_545 1_545 ?
O3 Na1 O3 180.0 . 7_656 ?
O3 Na1 O3 94.80(5) . 1_545 ?
O3 Na1 O3 180.0 7_666 1_545 ?
O3 Na1 O3 85.20(5) . 7_666 ?
O3 Na1 O3 85.20(5) 7_656 1_545 ?
O3 Na1 O3 94.80(5) 7_656 7_666 ?
O3 Na1 N1 88.1(3) 7_656 . ?
O3 Na1 N1 91.9(2) . . ?
O3 Na1 N1 91.9(3) 7_666 . ?
O3 Na1 N1 88.1(3) 1_545 . ?
N1 Na1 Na1 92.6(3) . 1_565 ?
N1 Na1 Na1 87.4(3) . 1_545 ?
Na1 O3 Na1 94.80(5) . 1_565 ?
N2 N1 Na1 118.8(6) . . ?
N4 N1 Na1 125.2(9) . . ?
N4 N1 N2 109.4(10) . . ?
C1 N2 N1 102.9(5) . . ?
C1 N3 N4 103.5(4) . . ?
N3 N4 N1 109.4(9) . . ?
O2 N5 C1 117.3(5) . . ?
N2 C1 N5 121.6(3) . . ?
N3 C1 N2 114.73(18) . . ?
N3 C1 N5 123.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 Na1 3.50530(19) 1_565 ?
Na1 Na1 3.5053(2) 1_545 ?
Na1 O1 2.372(10) . ?
Na1 O3 2.3747(13) . ?
Na1 O3 2.3872(13) 1_545 ?
Na1 O3 2.3747(13) 7_656 ?
Na1 O3 2.3872(13) 7_666 ?
Na1 N1 2.573(12) . ?
O2 N5 1.231(7) . ?
O3 Na1 2.3872(12) 1_565 ?
N1 N2 1.347(13) . ?
N1 N4 1.346(11) . ?
N2 C1 1.338(3) . ?
N3 N4 1.342(9) . ?
N3 C1 1.322(3) . ?
N5 C1 1.447(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O4 0.839(18) 1.969(18) 2.7988(18) 170(3) 4_656
O3 H3B O4 0.858(19) 1.97(2) 2.8139(18) 169(4) .
O4 H4A N2 0.87 2.03 2.803(3) 146.8 .
