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_7044477
_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)3, B4 O9 H4 2-, H2 O'
_chemical_formula_sum            'B4 H15 N3 O10 Zn'
_chemical_formula_weight         325.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-02-13 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.323(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.215(4)
_cell_length_b                   7.845(3)
_cell_length_c                   12.172(4)
_cell_measurement_reflns_used    2185
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.974
_cell_measurement_theta_min      3.135
_cell_volume                     1113.5(7)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.925
_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  0.0184
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5167
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.199
_diffrn_reflns_theta_min         3.130
_diffrn_source                   'Mo Sealed Tube'
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_recrystallization_method 'vapour diffusion '
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.166
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.281(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3344
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.562
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0396P)^2^+0.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                3033
_reflns_number_total             3344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03186f2.cif
_cod_data_source_block           ZnNH33tetraborato_E1
_cod_original_cell_volume        1113.5(6)
_cod_database_code               7044477
_shelx_estimated_absorpt_t_min   0.641
_shelx_estimated_absorpt_t_max   0.706
_shelxl_version_number           2014-3
_shelx_res_checksum              68418