#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011928.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7011928
loop_
_publ_author_name
'Teresa Avilés'
'António Dinis'
'José Orlando Gonçalves'
'Vitor Félix'
'Maria José Calhorda'
'Ângela Prazeres'
'Michael G. B. Drew'
'Helena Alves'
'Rui T. Henriques'
'Vasco da Gama'
'Piero Zanello'
'Marco Fontani'
_publ_section_title
;
 Synthesis, X-ray structures, electrochemistry, magnetic properties,
 and theoretical studies of the novel monomeric [CoI2(dppfO2)] and
 polymeric chain [CoI2(μ-dppfO2)n]
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4595
_journal_page_last               4602
_journal_paper_doi               10.1039/b205942h
_journal_year                    2002
_chemical_formula_sum            'C32 H26 N2 O6'
_chemical_formula_weight         534.55
_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                83.523(2)
_cell_angle_beta                 80.3840(10)
_cell_angle_gamma                87.233(2)
_cell_formula_units_Z            1
_cell_length_a                   6.1009(7)
_cell_length_b                   8.0739(9)
_cell_length_c                   13.4904(15)
_cell_measurement_reflns_used    1696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     650.70(13)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_method       'ω 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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4072
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.0837
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'thin plates'
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.043(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0746P)²+0.0485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                1582
_reflns_number_total             2441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205942h.txt
_cod_data_source_block           1.bipy
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011928
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.1566(3) 0.3332(2) 0.33224(13) 0.0669(5) Uani 1 1 d . . .
H1 H -0.206(5) 0.440(4) 0.358(2) 0.100(10) Uiso 1 1 d . . .
O2 O 0.1552(3) 0.4649(2) 0.27436(15) 0.0729(5) Uani 1 1 d . . .
O3 O 0.6852(3) 0.2694(2) 0.08550(13) 0.0654(5) Uani 1 1 d . . .
N1 N -0.3102(3) 0.6166(2) 0.40629(15) 0.0622(6) Uani 1 1 d . . .
C1 C -0.2030(5) 0.6895(3) 0.4662(2) 0.0840(9) Uani 1 1 d . . .
H1A H -0.0730 0.6375 0.4832 0.101 Uiso 1 1 calc R . .
C2 C -0.2714(5) 0.8368(3) 0.5048(2) 0.0768(8) Uani 1 1 d . . .
H2 H -0.1897 0.8807 0.5474 0.092 Uiso 1 1 calc R . .
C3 C -0.4602(3) 0.9194(3) 0.48057(14) 0.0462(5) Uani 1 1 d . . .
C4 C -0.5685(4) 0.8455(3) 0.4158(2) 0.0683(7) Uani 1 1 d . . .
H4 H -0.6956 0.8971 0.3953 0.082 Uiso 1 1 calc R . .
C5 C -0.4906(4) 0.6968(3) 0.3815(2) 0.0724(8) Uani 1 1 d . . .
H5 H -0.5687 0.6499 0.3386 0.087 Uiso 1 1 calc R . .
C6 C 0.0472(4) 0.3417(3) 0.28101(15) 0.0480(5) Uani 1 1 d . . .
C7 C 0.1287(3) 0.1850(3) 0.23639(14) 0.0427(5) Uani 1 1 d . . .
C8 C -0.0085(4) 0.0485(3) 0.25383(16) 0.0529(6) Uani 1 1 d . . .
H8 H -0.1498 0.0578 0.2917 0.063 Uiso 1 1 calc R . .
C9 C 0.0610(4) -0.1002(3) 0.21606(18) 0.0624(7) Uani 1 1 d . . .
H9 H -0.0323 -0.1905 0.2287 0.075 Uiso 1 1 calc R . .
C10 C 0.2683(4) -0.1139(3) 0.15990(18) 0.0625(7) Uani 1 1 d . . .
H10 H 0.3165 -0.2142 0.1345 0.075 Uiso 1 1 calc R . .
C11 C 0.4061(4) 0.0204(3) 0.14079(17) 0.0557(6) Uani 1 1 d . . .
H11 H 0.5463 0.0091 0.1022 0.067 Uiso 1 1 calc R . .
C12 C 0.3412(3) 0.1718(3) 0.17754(14) 0.0441(5) Uani 1 1 d . . .
C13 C 0.4911(3) 0.3188(3) 0.15123(16) 0.0507(6) Uani 1 1 d . . .
H13A H 0.4150 0.4118 0.1180 0.061 Uiso 1 1 calc R . .
H13B H 0.5316 0.3533 0.2121 0.061 Uiso 1 1 calc R . .
C14 C 0.8370(3) 0.3893(3) 0.04588(16) 0.0504(6) Uani 1 1 d . . .
C15 C 0.8097(4) 0.5567(3) 0.05861(16) 0.0550(6) Uani 1 1 d . . .
H15 H 0.6822 0.5956 0.0982 0.066 Uiso 1 1 calc R . .
C16 C 0.9717(4) 0.6665(3) 0.01250(17) 0.0552(6) Uani 1 1 d . . .
H16 H 0.9518 0.7793 0.0208 0.066 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 O3 C13 117.61(17) . . ?
C1 N1 C5 116.0(2) . . ?
N1 C1 C2 124.2(2) . . ?
C1 C2 C3 120.1(2) . . ?
C2 C3 C4 115.7(2) . . ?
C2 C3 C3 122.2(2) . 2_476 ?
C4 C3 C3 122.1(2) . 2_476 ?
C5 C4 C3 120.6(2) . . ?
N1 C5 C4 123.4(2) . . ?
O2 C6 O1 121.8(2) . . ?
O2 C6 C7 124.6(2) . . ?
O1 C6 C7 113.6(2) . . ?
C8 C7 C12 119.39(19) . . ?
C8 C7 C6 119.00(19) . . ?
C12 C7 C6 121.61(19) . . ?
C9 C8 C7 121.2(2) . . ?
C10 C9 C8 119.5(2) . . ?
C9 C10 C11 120.2(2) . . ?
C10 C11 C12 121.7(2) . . ?
C11 C12 C7 117.9(2) . . ?
C11 C12 C13 120.50(18) . . ?
C7 C12 C13 121.54(18) . . ?
O3 C13 C12 108.09(17) . . ?
O3 C14 C15 125.25(19) . . ?
O3 C14 C16 115.5(2) . 2_765 ?
C15 C14 C16 119.2(2) . 2_765 ?
C16 C15 C14 120.0(2) . . ?
C15 C16 C14 120.8(2) . 2_765 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C6 1.318(3) . ?
O2 C6 1.207(3) . ?
O3 C14 1.373(3) . ?
O3 C13 1.425(2) . ?
N1 C1 1.322(3) . ?
N1 C5 1.322(3) . ?
C1 C2 1.371(3) . ?
C2 C3 1.371(3) . ?
C3 C4 1.379(3) . ?
C3 C3 1.488(4) 2_476 ?
C4 C5 1.371(3) . ?
C6 C7 1.490(3) . ?
C7 C8 1.392(3) . ?
C7 C12 1.409(3) . ?
C8 C9 1.377(3) . ?
C9 C10 1.368(3) . ?
C10 C11 1.379(3) . ?
C11 C12 1.386(3) . ?
C12 C13 1.507(3) . ?
C14 C15 1.381(3) . ?
C14 C16 1.381(3) 2_765 ?
C15 C16 1.380(3) . ?
C16 C14 1.381(3) 2_765 ?
