Zn-OH2 and Zn-OH complexes with hydroborate-derived tripod ligands: a comprehensive study.
Ibrahim, Mohamed M.; Olmo, Cristina Pérez; Tekeste, Teame; Seebacher, Jan; He, Guosen; Maldonado Calvo, José A; Böhmerle, Karin; Steinfeld, Gunther; Brombacher, Horst; Vahrenkamp, Heinrich; Inorganic chemistry 45 (2006) 7493–7502; doi:10.1021/ic060752f

data_4350386
_publ_section_title
;
 Zn-OH2 and Zn-OH complexes with hydroborate-derived tripod ligands: a
 comprehensive study.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7493
_journal_page_last               7502
_journal_paper_doi               10.1021/ic060752f
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C48 H41 B2 N12 O7 Zn2, Cl O4'
_chemical_formula_sum            'C48 H45 B2 Cl N12 O11 Zn2'
_chemical_formula_weight         1153.76
_chemical_melting_point          216&#x00B0;C
_chemical_name_common
'complex 10 (Maldonado) [(TpFu,MeZn)2(OH)](ClO4)'
_chemical_name_systematic
; 
 Bis(hydrotris(3-(2&#x0092;-furyl)-5-methylpyrazol-1-yl)borate zinc) hydroxyde
;
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     PATT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.786(2)
_cell_length_b                   11.786(2)
_cell_length_c                   31.507(8)
_cell_measurement_temperature    247(2)
_cell_volume                     3790.3(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      247(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            11407
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1773
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          1.072
_refine_ls_shift/su_mean         0.253
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+10.9564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1816
_reflns_number_gt                2738
_reflns_number_total             4047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060752fsi20060504_033957.cif
_cod_data_source_block           josefm
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '-26(2)' was changed to
'247(2)' -- it was converted from degrees Celsius(C) to Kelvins(K).

data item '_geom_angle_publ_flag' value 'Y' was changed to 'y' in
accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (107 times).

data item '_geom_bond_publ_flag' value 'Y' was changed to 'y' in
accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (52 times).

data item '_symmetry_cell_setting' value 'Rhombohedral' was changed
to 'rhombohedral' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3790.1(13)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4350386