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_4312931
_publ_contact_author
;
         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            'C64 H82 Br4 N2 Ni2 O4.5 P2'
_chemical_formula_weight         1450.32
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.0980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.0209(3)
_cell_length_b                   17.5667(3)
_cell_length_c                   18.3020(3)
_cell_measurement_temperature    183(2)
_cell_volume                     6653.65(19)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_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)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            88822
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    3.062
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_type   semi-emperical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         15202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+13.5951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                10464
_reflns_number_total             15202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020534w_4.cif
_cod_data_source_block           FO1377
_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 
;
_cod_original_cell_volume        6653.65(18)
_cod_original_formula_sum        'C64 H82 Br4 N2 Ni2 O4.50 P2'
_cod_database_code               4312931