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_4350380
_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         'c54 H51 B2 N18 O2 Zn2, C H4 O, H2 O, Cl2 O8'
_chemical_formula_sum            'C55 H57 B2 Cl2 N18 O12 Zn2'
_chemical_formula_weight         1385.45
_chemical_melting_point          '300 &#x00B0;C'
_chemical_name_common
'Complex 2 (Perez), [Tp4&#x0091;Py,MeZn&#x00B7;OH2]ClO4'
_chemical_name_systematic
; 
 Hydrotris(3-(4&#x0091;-pyridyl)-5-methyl)pyrazolylborate  zinc  aqua perchlorate 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.907(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.312(6)
_cell_length_b                   11.316(2)
_cell_length_c                   25.932(6)
_cell_measurement_temperature    247(2)
_cell_volume                     7213(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      247(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.1492
_diffrn_reflns_av_sigmaI/netI    0.2241
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            63184
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.783
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         17506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.783
_refine_ls_R_factor_all          0.1925
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.527
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1975
_refine_ls_wR_factor_ref         0.2350
_reflns_number_gt                5382
_reflns_number_total             17506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060752fsi20060504_033957.cif
_cod_data_source_block           crijm
_cod_depositor_comments
;
The following automatic conversions were performed:

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 (168 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 (106 times).

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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_sg_symbol_H-M      P2(1)/c
_cod_database_code               4350380