Multitopic third generation tris(pyrazolyl)methane ligands built on alkyne structural scaffolding: first preparation of mixed tris(pyrazolyl)methane/tris(pyrazolyl)borate ligands
Daniel L. Reger; James R. Gardinier; Selma Bakbak; Radu F. Semeniuc; Uwe H. F. Bunz; Mark D. Smith; New Journal of Chemistry 29 (2005) 1035–; doi:10.1039/b414770g

data_7050055
_publ_section_title
;
 Multitopic third generation tris(pyrazolyl)methane ligands built on
 alkyne structural scaffolding: first preparation of mixed
 tris(pyrazolyl)methane/tris(pyrazolyl)borate ligands
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1035
_journal_paper_doi               10.1039/b414770g
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C58 H52 B2 Fe N24 O2, 4 C H2 CL2'
_chemical_formula_sum            'C62 H60 B2 Cl8 Fe N24 O2'
_chemical_formula_weight         1534.41
_chemical_name_systematic
;
?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.9530(10)
_cell_angle_beta                 98.3300(10)
_cell_angle_gamma                106.9990(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5941(4)
_cell_length_b                   13.4373(7)
_cell_length_c                   16.3188(8)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26.380
_cell_measurement_theta_min      2.413
_cell_volume                     1701.27(15)
_computing_cell_refinement       'SAINT+ NT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 1998)'
_computing_data_reduction        'SAINT+ NT V6.22'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16083
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.882
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_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1557P)^2^+0.3511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2232
_reflns_number_gt                4840
_reflns_number_total             5990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414770g.txt
_cod_data_source_block           sqz
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1701.26(15)
_cod_database_code               7050055