Zinc hydridotriphenylborates suppported by a neutral macrocyclic polyamine
Okuda, Jun; Mukherjee, Debabarata; Spaniol, Thomas Paul; Wiegand, Ann-Kristin; Dalton Trans.  (2017) –; doi:10.1039/C7DT01094J

data_7042712
_publ_section_title
;
 Zinc hydridotriphenylborates suppported by a neutral macrocyclic
 polyamine
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01094J
_journal_year                    2017
_chemical_formula_moiety         '2(C12 H28 I N4 Zn), 3(C4 H8 O), 2(I)'
_chemical_formula_sum            'C36 H80 I4 N8 O3 Zn2'
_chemical_formula_weight         1311.42
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.987(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.936(2)
_cell_length_b                   12.276(3)
_cell_length_c                   25.751(7)
_cell_measurement_reflns_used    1674
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.29
_cell_measurement_theta_min      2.63
_cell_volume                     2499.2(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.1152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22658
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.483
_diffrn_reflns_theta_min         1.588
_exptl_absorpt_coefficient_mu    3.470
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       rod
_exptl_crystal_F_000             1296
_exptl_crystal_recrystallization_method
'reactive crystallization from thf at room temperature'
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5153
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0331P)^2^+3.4017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3429
_reflns_number_total             5153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01094j2.cif
_cod_data_source_block           4
_cod_database_code               7042712
_shelx_estimated_absorpt_t_min   0.466
_shelx_estimated_absorpt_t_max   0.607
_shelxl_version_number           2013-4
_shelx_res_checksum              80366