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_4312932
_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
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_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
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 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            'C44 H42 Br2 N2 Ni P2'
_chemical_formula_weight         879.27
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.304(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3600(3)
_cell_length_b                   11.0980(1)
_cell_length_c                   17.9282(2)
_cell_measurement_temperature    120(2)
_cell_volume                     3846.01(8)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_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      120(2)
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'SMART - Bruker'
_diffrn_measurement_method       phi-scan
_diffrn_radiation_monochromator  SI<111>
_diffrn_radiation_source         'synchrotron - ESRF'
_diffrn_radiation_wavelength     0.45085
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25156
_diffrn_reflns_theta_full        14.51
_diffrn_reflns_theta_max         14.51
_diffrn_reflns_theta_min         7.20
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9165
_exptl_absorpt_correction_type   ?semi-empirical
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.221(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    rigid-group
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         4692
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.2422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                4654
_reflns_number_total             4692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020534w_5.cif
_cod_data_source_block           FO1402
_cod_depositor_comments
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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 
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_cod_database_code               4312932