Synthesis, Spectroscopic Characterization, and Crystal Structure of the Bimetallic Complex [Ni2(μ-CO)(CO)2(μ-NH(PPh2)2)2]
Eugenio Simón-Manso; Mauricio Valderrama; Verónica Arancibia; Yamil Simón-Manso; Daphne Boys; Inorganic Chemistry 39 (2000) 1650–1654; doi:10.1021/ic990773s

data_4320858
_publ_section_title
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 Synthesis, Spectroscopic Characterization, and Crystal Structure of the
 Bimetallic Complex [Ni2(\m-CO)(CO)2(\m-NH(PPh2)2)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1650
_journal_page_last               1654
_journal_paper_doi               10.1021/ic990773s
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'Ni2 C O (C O)2 (Ph2 P N H P Ph2)2'
_chemical_formula_structural     'Ni2 C O (C O)2 (Ph2 P N H P Ph2)2'
_chemical_formula_sum            'C51 H42 N2 Ni2 O3 P4'
_chemical_formula_weight         972.17
_chemical_name_systematic
;
 \m-Carbonyl-bis-\m-[bis(diphenylphosphino)amine]-bis(carbonyl nickel)
;
_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
_cell_angle_alpha                79.91(1)
_cell_angle_beta                 79.96(1)
_cell_angle_gamma                71.32(1)
_cell_formula_units_Z            2
_cell_length_a                   13.009(1)
_cell_length_b                   13.063(2)
_cell_length_c                   14.664(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      4
_cell_volume                     2305.4(5)
_computing_cell_refinement       'Siemens P3/P4-PC version V4.27'
_computing_data_collection       'Siemens P3/P4-PC version V4.27'
_computing_data_reduction        'XDISK in SHELXTL/PC'
_computing_molecular_graphics    'XP in SHELXTL/PC'
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    'XS in SHELXTL-PC'
_diffrn_ambient_temperature      297(2)
_diffrn_measurement_device_type  'Siemens R3m/V 4-circle diffractometer'
_diffrn_measurement_method       '\q/2\q 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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10936
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10118
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                6156
_reflns_number_total             10119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990773s.cif
_cod_data_source_block           nip
_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^)+(0.0536P)^2^+0.0000P] 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^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320858