Selective synthesis of U-shaped terpyridines. Versatile ligands for the preparation of platinum complexes.
Sielemann, Dirk; Winter, Andreas; Flörke, Ulrich; Risch, Nikolaus; Organic & biomolecular chemistry 2 (2004) 863–868; doi:10.1039/b316633c

data_7150361
_publ_section_title
;
 Selective synthesis of U-shaped terpyridines. Versatile ligands for
 the preparation of platinum complexes.
;
_journal_issue                   6
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              863
_journal_page_last               868
_journal_paper_doi               10.1039/b316633c
_journal_volume                  2
_journal_year                    2004
_chemical_formula_moiety         '(C32 H28 N4 O Pt)(B F4)2 * 2 CH3CN'
_chemical_formula_sum            'C36 H34 B2 F8 N6 O Pt'
_chemical_formula_weight         935.40
_chemical_name_common            'C36 H34 B2 F8 N6 O1 Pt1'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.90(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.275(4)
_cell_length_b                   8.415(3)
_cell_length_c                   23.953(5)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15.658
_cell_measurement_theta_min      6.143
_cell_volume                     3604.8(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7818
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        6
_diffrn_standards_interval_count 397
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.974
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.372
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6263
_refine_ls_number_restraints     835
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.131
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                4428
_reflns_number_total             6263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b316633c.txt
_cod_data_source_block           14e
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7150361