Dicopper(I) Complexes with Reduced States of 3,6-Bis(2'-pyrimidyl)-1,2,4,5-tetrazine: Crystal Structures and Spectroscopic Properties of the Free Ligand, a Radical Species, and a Complex of the 1,4-Dihydro Form
Markus Glöckle; Klaus Hübler; Hans-Jürgen Kümmerer; Gert Denninger; Wolfgang Kaim; Inorganic Chemistry 40 (2001) 2263–2269; doi:10.1021/ic001228q

data_4319628
_publ_contact_author
;
   Prof. Dr. W. Kaim
   Institut f\"ur Anorganische Chemie
   Universit\"at Stuttgart
   Pfaffenwaldring 55
   D-70550 Stuttgart
   Germany
;
_publ_contact_author_email       kaim@iac.uni-stuttgart.de
_publ_contact_author_fax         '049 711 685-4165'
_publ_contact_author_phone       '049 711 685-4171'
_publ_section_title
;
 Dicopper(I) Complexes with Reduced States of
 3,6-Bis(2'-pyrimidyl)-1,2,4,5-tetrazine: Crystal Structures and
 Spectroscopic Properties of the Free Ligand, a Radical Species, and a
 Complex of the 1,4-Dihydro Form
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2263
_journal_page_last               2269
_journal_paper_doi               10.1021/ic001228q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C83 H70 B2 Cl2 Cu2 F8 N8 P4'
_chemical_formula_weight         1674.95
_chemical_name_common            '{(mu-H2bmtz)[Cu(Ph3)2]2}(BF4)2 . CH2Cl2'
_chemical_name_systematic
;
(mu-(1,4-dihydro-3,6-bis(2'-pyrimidyl)-1,2,4,5-tetrazine))
bis[bis(triphenylphosphane)copper(I)]
bis(tetrafluoroborate)-dichloromethane solvate
;
_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                93.82(3)
_cell_angle_beta                 94.46(3)
_cell_angle_gamma                101.60(3)
_cell_formula_units_Z            2
_cell_length_a                   10.948(2)
_cell_length_b                   12.067(2)
_cell_length_c                   30.287(6)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.30
_cell_measurement_theta_min      7.51
_cell_volume                     3893.7(13)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P3'
_diffrn_measurement_method       Wyckoff
_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  0.0940
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12937
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.73
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.8936
_exptl_absorpt_correction_T_min  0.7489
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'bright orange'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         12213
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1952
_reflns_number_gt                7446
_reflns_number_total             12213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001228q_3.cif
_cod_data_source_block           {(mu-H2bmtz)[Cu(Ph3)2]2}(BF4)2.CH2Cl2
_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:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        3893.8(14)
_cod_database_code               4319628