Synthesis and characterization of Co and Ni complexes stabilized by keto- and acetamide-derived P,O-type phosphine ligands
Agostinho, Magno; Rosa, Vitor; Avilés, Teresa; Welter, Richard; Braunstein, Pierre; Dalton Transactions  (2009) 814–822; doi:10.1039/b814284j

data_7000392
_publ_section_title
;
 Synthesis and characterization of Co and Ni complexes stabilized by
 keto- and acetamide-derived P,O-type phosphine ligands
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              814
_journal_page_last               822
_journal_paper_doi               10.1039/b814284j
_journal_year                    2009
_chemical_formula_moiety         '2(C19 H18 Co I2 N O P), 3/2(C H2 Cl2)'
_chemical_formula_sum            'C39.5 H39 Cl3 Co2 I4 N2 O2 P2'
_chemical_formula_weight         1367.48
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                89.393(2)
_cell_angle_beta                 82.027(2)
_cell_angle_gamma                76.3740(14)
_cell_formula_units_Z            2
_cell_length_a                   8.0520(3)
_cell_length_b                   15.4070(5)
_cell_length_c                   19.8740(7)
_cell_measurement_reflns_used    7323
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2372.33(15)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f 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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19144
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    3.573
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1306
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.977
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         13854
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+6.7228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1971
_reflns_number_gt                8377
_reflns_number_total             13854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814284j.txt
_cod_data_source_block           complex_5
_cod_original_cell_volume        2372.33(14)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C39.50 H39 Cl3 Co2 I4 N2 O2 P2'
_cod_database_code               7000392