Preparation and characterization of mixed-ligand cobalt(III) complexes containing (3-aminopropyl)dimethylphosphine (pdmp). Conformation of the six-membered pdmp chelate ring.
Suzuki, Takayoshi; Fujiiwara, Katsuhiro; Takagi, Hideo D.; Kashiwabara, Kazuo; Dalton transactions (Cambridge, England : 2003)  (2007) 308–319; doi:10.1039/b612025c

data_7004859
_publ_section_title
;
 Preparation and characterization of mixed-ligand cobalt(III) complexes
 containing (3-aminopropyl)dimethylphosphine (pdmp). Conformation of
 the six-membered pdmp chelate ring.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              308
_journal_page_last               319
_journal_paper_doi               10.1039/b612025c
_journal_year                    2007
_chemical_formula_moiety
'C15 H35 Co N2 O2 P2 2+, 2(F6 P 1-), 0.5(C4 H10 O)'
_chemical_formula_sum            'C17 H40 Co F12 N2 O2.5 P4'
_chemical_formula_weight         723.32
_chemical_name_common
;
trans(P,N)-(pentane-2,4-dionato)bis((3-aminopropyl)
dimethylphosphine)cobalt(iii) Bis(hexafluorophospate) Hemi(diethyl
ether) Solvate
;
_chemical_name_systematic
;
trans(P,N)-(pentane-2,4-dionato)bis((3-aminopropyl)
dimethylphosphine)cobalt(III) Bis(hexafluorophospate)
Hemi(diethyl ether) Solvate
;
_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                 94.258(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.765(5)
_cell_length_b                   11.701(3)
_cell_length_c                   31.311(10)
_cell_measurement_reflns_used    26557
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     6125(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'CrystalStructure 3.7.0'
_computing_molecular_graphics    'ORTEP-3 for Win'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            53373
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.8463
_exptl_absorpt_correction_T_min  0.8131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            octahedron
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         13967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+4.6916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1751
_reflns_number_gt                9602
_reflns_number_total             13967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b612025c.txt
_cod_data_source_block           transPN
_cod_original_formula_sum        'C17 H40 Co F12 N2 O2.50 P4'
_cod_database_code               7004859