Synthesis, structural characterization and scalable preparation of new amino-zinc borates.
Imer, Marcos Ramón; González, Mariana Estefani; Veiga, Nicolás; Kremer, Carlos; Suescun, Leopoldo; Arizaga, Livia; Dalton Trans.  (2017) –; doi:10.1039/C7DT03186F

data_7044478
_publ_section_title
;
 Synthesis, structural characterization and scalable preparation of new
 amino-zinc borates.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03186F
_journal_year                    2017
_chemical_formula_moiety         'Zn 2+, (N H3)4, B4 O9 H4 2-, (H2 O)4'
_chemical_formula_sum            'B4 H24 N4 O13 Zn'
_chemical_formula_weight         396.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-13 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0796(9)
_cell_length_b                   11.8853(5)
_cell_length_c                   16.7606(8)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.195
_cell_measurement_theta_min      2.784
_cell_volume                     3003.9(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\j and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100416
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.616
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'Mo Sealed Tube'
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       'capped octahedra'
_exptl_crystal_F_000             1648
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diluted ammonium hydroxide in water'
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.195
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      3.564
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+2.0035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3806
_reflns_number_total             4605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03186f2.cif
_cod_data_source_block           ZnNH34tetraborato_E2_final
_cod_database_code               7044478
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.732
_shelx_res_checksum              7956