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_7050053
_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_sum            'C30 H29 I N12 O2'
_chemical_formula_weight         716.55
_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                96.8400(10)
_cell_angle_beta                 99.5630(10)
_cell_angle_gamma                105.9950(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7819(6)
_cell_length_b                   12.1248(8)
_cell_length_c                   15.3073(10)
_cell_measurement_reflns_used    5607
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.382
_cell_measurement_theta_min      2.560
_cell_volume                     1521.48(18)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0442
_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            13447
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.748
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.0387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                5688
_reflns_number_total             6156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414770g.txt
_cod_data_source_block           sb176m
_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_sg_symbol_H-M      P-1
_cod_database_code               7050053