NaK15[B4O5(OH)4]6(NO2)2(CO3)·7H2O: assembly of an unprecedented mixed anion inorganic compound via a facile hydrothermal route
Cao, Yuchen; Zhang, Bingbing; Liu, Hongkun; Li, Danni; Wang, Ying; New Journal of Chemistry 44 (2020) 4253–4256; doi:10.1039/D0NJ00249F

data_7059326
_publ_section_title
;
 NaK15[B4O5(OH)4]6(NO2)2(CO3)&#x00B7;7H2O: assembly of an unprecedented
 mixed anion inorganic compound via a facile hydrothermal route
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4253
_journal_page_last               4256
_journal_paper_doi               10.1039/D0NJ00249F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '0.5(C2 H76 B48 K30 N4 Na2 O136)'
_chemical_formula_sum            'C H38 B24 K15 N2 Na O68'
_chemical_formula_weight         2035.26
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-09 deposited with the CCDC.	2020-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   11.1399(9)
_cell_length_b                   11.1399(9)
_cell_length_c                   30.495(5)
_cell_measurement_reflns_used    4358
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.50
_cell_volume                     3277.3(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       '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      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            23200
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         0.668
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0556 before and 0.0504 after correction. The Ratio of minimum to maximum transmission is 0.9275. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 906 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2576
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0446P)^2^+1.1916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2295
_reflns_number_total             2576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00249f2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7059326.cif.

 Adding full bibliography for 7059326.cif.
;
_cod_database_code               7059326
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.61(7)
 0.39(7)
2. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
3. Restrained distances
 O13-H13 = O5-H5 = O12-H12 = O8-H8 = O1-H1 = O9-H9 = O10-H10
 0.88 with sigma of 0.02
 N1-O17
 1.15 with sigma of 0.02
 O16-O17
 2.05 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of
0.003 and sigma for terminal atoms of 0.006
5. Others
 Sof(O16)=0.33333*(1-FVAR(2))
 Sof(O17)=0.3333*(1-FVAR(2))
 Sof(O14)=Sof(O15)=0.33333*FVAR(2)
 Fixed Sof: O10(0.16667) H10(0.33333)
;
_shelx_res_checksum              30610
_olex2_submission_special_instructions 'No special instructions were received'