Pyrazolylborate-Zinc-Nucleobase-Complexes, 2:1 Preparations and Structures of TpCum,MeZn and TpPh,MeZn Complexes
Dirk Badura; Heinrich Vahrenkamp; Inorganic Chemistry 41 (2002) 6013–6019; doi:10.1021/ic020280e

data_4318817
_publ_section_title
;
 Pyrazolylborate-Zinc-Nucleobase-Complexes, 2:1 Preparations and
 Structures of TpCum,MeZn and TpPh,MeZn Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6013
_journal_page_last               6019
_journal_paper_doi               10.1021/ic020280e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C70 H72 B2 Cl2 N16 O5 Zn2'
_chemical_formula_weight         1440.70
_chemical_name_common            TpPh,MeZn-DHU
_chemical_name_systematic
;
Hydrotris(5-methyl-3-phenyl-pyrazol-1-yl)borato-zink-dihydrouraCilat
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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                 104.747(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7136(19)
_cell_length_b                   17.535(2)
_cell_length_c                   25.347(3)
_cell_measurement_temperature    180(2)
_cell_volume                     6754.0(14)
_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      180(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area deteCtor'
_diffrn_measurement_method       'phi and omega sCans'
_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  0.2704
_diffrn_reflns_av_sigmaI/netI    0.3182
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61269
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometriC
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.311
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.0097(7)
_refine_ls_extinction_expression FC^*^=kFC[1+0.001xFC^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    'Riding Model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         16404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.3452
_refine_ls_R_factor_gt           0.1046
_refine_ls_shift/su_max          2.846
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'CalC w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2329
_refine_ls_wR_factor_ref         0.3421
_reflns_number_gt                4451
_reflns_number_total             16404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020280e_4.cif
_cod_data_source_block           dhut
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_primary' value 'direCt' changed to
'direct' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'CalC' changed to
'calc' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_site_calc_flag'
value 'CalC' changed to 'calc' according to the built-in table from
CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29 (72 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318817