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_4318816
_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            'C37.5 H41.5 B N12 O2.5 Zn'
_chemical_formula_weight         776.51
_chemical_name_common            TpPh,MeZn-DAP
_chemical_name_systematic
;
Hydrotris(5-methyl-3-phenyl-pyrazol-1-yl)borato-zinc-diaminopurinat
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.28(3)
_cell_angle_beta                 102.33(3)
_cell_angle_gamma                97.69(3)
_cell_formula_units_Z            2
_cell_length_a                   12.394(3)
_cell_length_b                   12.793(3)
_cell_length_c                   13.099(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1893.6(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  NONIUS-TURBO-CAD4
_diffrn_measurement_method       '\w-2theta 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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7794
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.54
_diffrn_standards_interval_count 'OCR every 200 refl.'
_diffrn_standards_interval_time  'ICR every 7200 refl.'
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             811
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+1.3296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                6104
_reflns_number_total             7441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020280e_3.cif
_cod_data_source_block           b1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1893.6(7)
_cod_original_formula_sum        'C37.50 H41.50 B N12 O2.50 Zn'
_cod_database_code               4318816