Chloride Ion-Aided Self-Assembly of Pseudoclathrochelate Metal Tris-pyrazoloximates.
Varzatskii, Oleg A.; Penkova, Larysa V.; Kats, Svitlana V.; Dolganov, Alexander V.; Vologzhanina, Anna V.; Pavlov, Alexander A.; Novikov, Valentin V.; Bogomyakov, Artem S.; Nemykin, Victor N.; Voloshin, Yan Z.; Inorganic chemistry 53 (2014) 3062–3071; doi:10.1021/ic4029047

data_4337704
_publ_section_title
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 Chloride Ion-Aided Self-Assembly of Pseudoclathrochelate Metal
 Tris-pyrazoloximates.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3062
_journal_page_last               3071
_journal_paper_doi               10.1021/ic4029047
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C21 H23 B N9 O3 Zn 1+, Cl 1-, C H Cl3'
_chemical_formula_sum            'C22 H24 B Cl4 N9 O3 Zn'
_chemical_formula_weight         680.48
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 119.719(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.287(4)
_cell_length_b                   19.251(9)
_cell_length_c                   20.497(9)
_cell_measurement_reflns_used    1630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.41
_cell_volume                     2840(2)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14609
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6509
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                3796
_reflns_number_total             6509
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic4029047_si_002.cif
_cod_data_source_block           ZnPzOx
_cod_database_code               4337704
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3A(0.023) H6A(0.023) H9A(0.027) H1A(0.049) H1B(0.049) H1C(0.049)
 H4A(0.025) H5A(0.026) H6B(0.036) H6C(0.036) H6D(0.036) H9B(0.025) H10A(0.026)
 H11A(0.038) H11B(0.038) H11C(0.038) H14A(0.027) H15A(0.033) H17A(0.022)
 H18A(0.026) H19A(0.027) H20A(0.026) H21A(0.022) H22A(0.052)
 Fixed X: H3A(0.141) H6A(0.5307) H9A(0.4646) H1A(-0.3595) H1B(-0.4228) H1C(-
 0.3339) H4A(-0.3653) H5A(-0.1719) H6B(0.4678) H6C(0.6361) H6D(0.65)
 H9B(0.7721) H10A(0.7763) H11A(0.5448) H11B(0.3645) H11C(0.5556) H14A(0.6219)
 H15A(0.6257) H17A(0.0099) H18A(-0.0492) H19A(0.0386) H20A(0.181) H21A(0.2403)
 H22A(0.7556)
 Fixed Y: H3A(0.6365) H6A(0.7018) H9A(0.5537) H1A(0.6515) H1B(0.6127)
 H1C(0.5692) H4A(0.6075) H5A(0.6165) H6B(0.8071) H6C(0.7529) H6D(0.8197)
 H9B(0.8196) H10A(0.7842) H11A(0.4696) H11B(0.4251) H11C(0.4123) H14A(0.4023)
 H15A(0.4457) H17A(0.5292) H18A(0.521) H19A(0.6103) H20A(0.7102) H21A(0.7179)
 H22A(0.6295)
 Fixed Z: H3A(0.3549) H6A(0.4012) H9A(0.3969) H1A(0.0104) H1B(0.0631)
 H1C(0.0221) H4A(0.1871) H5A(0.3278) H6B(0.1028) H6C(0.1335) H6D(0.1825)
 H9B(0.3176) H10A(0.4368) H11A(0.124) H11B(0.1062) H11C(0.1826) H14A(0.3119)
 H15A(0.4289) H17A(-0.0681) H18A(-0.1909) H19A(-0.2431) H20A(-0.1723) H21A(-
 0.0486) H22A(0.5286)
;