The First Crystal Structure of a Metal-Stabilized Tetrazine Anion Radical: Formation of a Dicopper Complex through Self-Assembly in a Comproportionation Reaction
Manuela Schwach; Hans-Dieter Hausen; Wolfgang Kaim; Inorganic Chemistry 38 (1999) 2242–2243; doi:10.1021/ic9814625

data_4322023
_publ_contact_author
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       Prof.Dr.Wolfgang Kaim
       Institut f\"ur Anorganische Chemie
       Universit\"at Stuttgart             
       Pfaffenwaldring 55                  
       70569 Stuttgart                
       Bundesrepublik Deutschland
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_publ_contact_author_fax         '049 711 685-4241'
_publ_contact_author_phone       '049 711 685-4170'
_publ_section_title
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 The First Crystal Structure of a Metal-Stabilized Tetrazine Anion
 Radical: Formation of a Dicopper Complex through Self-Assembly in a
 Comproportionation Reaction
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2242
_journal_page_last               2243
_journal_paper_doi               10.1021/ic9814625
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural
;
[(Ph3P)2Cu(bptz)Cu(PPh3)2](BF4) with
 bptz= 3,6-bis(2-pyridyl)-1,2,4,5-tetrazine
;
_chemical_formula_sum            'C84 H68 B Cu2 F4 N6 P4'
_chemical_formula_weight         1499.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.076(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5968(11)
_cell_length_b                   16.7018(11)
_cell_length_c                   15.5733(7)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      1.5
_cell_volume                     3759.3(4)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6871
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_type   not
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       plates
_exptl_crystal_F_000             1546
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.443
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_obs          0.0616
_refine_ls_shift/esd_max         0.027
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+5.4357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1891
_refine_ls_wR_factor_obs         0.1653
_reflns_number_observed          4986
_reflns_number_total             6605
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9814625.cif
_cod_data_source_block           cubf
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+5.4357P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+5.4357P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322023