Metal Complexes with 2,3-Bis(diphenylphosphino)-1,4-diazadiene Ligands: Synthesis, Structures, and an Intramolecular Metal-Mediated [4 + 2] Cycloaddition Employing a Benzene Ring as a Dienophile
Dirk Walther; Stefan Liesicke; Lars Böttcher; Reinald Fischer; Helmar Görls; Gavin Vaughan; Inorganic Chemistry 42 (2003) 625–632; doi:10.1021/ic020534w

data_4312933
_publ_contact_author
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         Dirk Walther
         Friedrich-Schiller-Universit\"at Jena
         Institut f\"ur Anorganische und Analytische Chemie
         August-Bebel-Str. 2
         D-07743 Jena
         Germany
;
_publ_contact_author_email       'cdw@rz.uni-jena.de.de '
_publ_contact_author_fax         '03641 9-48102 '
_publ_contact_author_phone       '03641 9-48110 '
_publ_section_title
;
 Metal Complexes with 2,3-Bis(diphenylphosphino)-1,4-diazadiene Ligands:
 Synthesis, Structures, and an Intramolecular Metal-Mediated [4 + 2]
 Cycloaddition Employing a Benzene Ring as a Dienophile
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              625
_journal_page_last               632
_journal_paper_doi               10.1021/ic020534w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C54 H62 Br2 N2 Ni O2 P2'
_chemical_formula_weight         1051.53
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_cell_angle_alpha                90.00
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_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.571(2)
_cell_length_b                   14.2390(10)
_cell_length_c                   21.549(3)
_cell_measurement_temperature    183(2)
_cell_volume                     5505.1(12)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4-EXPRESS
_computing_data_reduction        MOLEN
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
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_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_av_sigmaI/netI    0.1365
_diffrn_reflns_limit_h_max       0
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_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.21
_diffrn_standards_interval_time  7200
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_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.8041
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_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1675
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
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_reflns_number_gt                5082
_reflns_number_total             9261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020534w_6.cif
_cod_data_source_block           FO1398
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        5505.1(10)
_cod_database_code               4312933