Solid-State Synthesis and Structure of the Enigmatic Ammonium Octaborate: (NH4)2[B7O9(OH)5]·3/4B(OH)3·5/4H2O.
Neiner, Doinita; Sevryugina, Yulia V.; Schubert, David M.; Inorganic chemistry 55 (2016) 8706–8711; doi:10.1021/acs.inorgchem.6b01243

data_4348501
_publ_section_title
;
 Solid-State Synthesis and Structure of the Enigmatic Ammonium Octaborate:
 (NH4)2[B7O9(OH)5]&#x00B7;3/4B(OH)3&#x00B7;5/4H2O.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8706
_journal_page_last               8711
_journal_paper_doi               10.1021/acs.inorgchem.6b01243
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
;
 {(N H4)2 B7 O9 (O H)5}4 B3 (O H )9 (H2 O)5
;
_chemical_formula_sum            'B31 H71 N8 O70'
_chemical_formula_weight         1638.75
_chemical_melting_point          ?
_chemical_name_systematic
;
 diammonium pentahydroxyheptaborate boric acid water solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.0915(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.41368(16)
_cell_length_b                   11.88771(19)
_cell_length_c                   23.4459(3)
_cell_measurement_reflns_used    29860
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.15
_cell_measurement_theta_min      3.76
_cell_volume                     3181.19(8)
_computing_cell_refinement
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'SHELXP (Sheldrick, 2008)'
_computing_publication_material  'SHELXCIF-2013/2 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59711
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.336
_diffrn_reflns_theta_min         3.718
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.509
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.482
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         6636
_refine_ls_number_restraints     630
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0515
_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^)+(0.1242P)^2^+2.0197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6460
_reflns_number_total             6636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01243_si_001.cif
_cod_data_source_block           {(NH4)2[B7O9(OH)5]}4(3B(OH)3)5H2O_(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348501
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.942
_shelxl_version_number           2014/6
_shelx_res_checksum              1993
_shelx_hkl_checksum              43761