#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011929.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_7011929
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            'C34 H28 N2 O6'
_chemical_formula_weight         560.58
_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                 91.627(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9416(11)
_cell_length_b                   8.1164(10)
_cell_length_c                   18.832(2)
_cell_measurement_reflns_used    1846
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      2.5
_cell_volume                     1366.2(3)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1267
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7674
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs (Sheldrick, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'distorted hexagonal block'
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2408
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0808
_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)+(0.1200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2080
_reflns_number_gt                1702
_reflns_number_total             2408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205942h.txt
_cod_data_source_block           197
_cod_original_cell_volume        1366.1(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011929
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.2968(2) 0.2097(3) 0.33875(9) 0.0535(6) Uani 1 1 d . . .
H1 H 0.3206 0.3007 0.3557 0.088(13) Uiso 1 1 calc R . .
O2 O 0.2805(3) 0.3533(2) 0.23810(11) 0.0610(7) Uani 1 1 d . . .
O3 O 0.1043(2) 0.2406(2) 0.08287(9) 0.0487(6) Uani 1 1 d . . .
N1 N 0.3563(9) 0.4861(6) 0.4063(3) 0.043(4) Uani 0.696(13) 1 d PD A 1
C1 C 0.2941(8) 0.5334(9) 0.4657(3) 0.044(3) Uani 0.696(13) 1 d PD A 1
H1A H 0.2230 0.4623 0.4850 0.052 Uiso 0.696(13) 1 calc PR A 1
C2 C 0.3237(7) 0.6757(7) 0.5013(3) 0.0469(13) Uani 0.696(13) 1 d PD A 1
H2 H 0.2731 0.7012 0.5429 0.056 Uiso 0.696(13) 1 calc PR A 1
C3 C 0.4297(6) 0.7827(5) 0.4753(3) 0.0378(12) Uani 0.696(13) 1 d PD A 1
C4 C 0.4998(6) 0.7337(6) 0.4139(4) 0.0435(13) Uani 0.696(13) 1 d PD A 1
H4 H 0.5745 0.7991 0.3939 0.052 Uiso 0.696(13) 1 calc PR A 1
C5 C 0.4572(8) 0.5878(7) 0.3833(4) 0.0503(17) Uani 0.696(13) 1 d PD A 1
H5 H 0.5053 0.5576 0.3415 0.060 Uiso 0.696(13) 1 calc PR A 1
C6 C 0.4621(5) 0.9379(5) 0.5115(2) 0.0445(16) Uani 0.696(13) 1 d PD . 1
H6 H 0.4234 0.9493 0.5571 0.053 Uiso 0.696(13) 1 calc PR A 1
N1A N 0.3659(18) 0.4806(13) 0.4088(8) 0.059(12) Uiso 0.304(13) 1 d PG A 2
C1A C 0.4738(14) 0.5618(13) 0.3702(6) 0.033(4) Uiso 0.304(13) 1 d PG A 2
H1A1 H 0.5133 0.5115 0.3298 0.039 Uiso 0.304(13) 1 calc PR A 2
C2A C 0.5231(10) 0.7172(12) 0.3912(5) 0.041(4) Uiso 0.304(13) 1 d PGD A 2
H2A H 0.5960 0.7720 0.3650 0.050 Uiso 0.304(13) 1 calc PR A 2
C3A C 0.4645(10) 0.7915(9) 0.4508(6) 0.027(3) Uiso 0.304(13) 1 d PGD A 2
C4A C 0.3567(12) 0.7104(13) 0.4894(6) 0.038(4) Uiso 0.304(13) 1 d PGD A 2
H4A H 0.3172 0.7606 0.5298 0.045 Uiso 0.304(13) 1 calc PR A 2
C5A C 0.3074(16) 0.5549(15) 0.4684(8) 0.074(12) Uiso 0.304(13) 1 d PG A 2
H5A H 0.2345 0.5001 0.4946 0.088 Uiso 0.304(13) 1 calc PR A 2
C6A C 0.5198(11) 0.9558(12) 0.4715(6) 0.043(4) Uiso 0.304(13) 1 d PD . 2
H6A H 0.5902 1.0042 0.4418 0.051 Uiso 0.304(13) 1 calc PR A 2
C7 C 0.2675(3) 0.2254(3) 0.27049(14) 0.0414(7) Uani 1 1 d . . .
C8 C 0.2199(3) 0.0663(3) 0.23621(13) 0.0374(6) Uani 1 1 d . . .
C9 C 0.2869(3) -0.0790(3) 0.26155(15) 0.0454(7) Uani 1 1 d . . .
H9 H 0.3561 -0.0739 0.3000 0.039(7) Uiso 1 1 calc R . .
C10 C 0.2533(4) -0.2289(3) 0.23117(15) 0.0515(8) Uani 1 1 d . . .
H10 H 0.3025 -0.3248 0.2473 0.063(9) Uiso 1 1 calc R . .
C11 C 0.1472(4) -0.2377(3) 0.17709(17) 0.0545(8) Uani 1 1 d . . .
H11 H 0.1216 -0.3403 0.1570 0.066(9) Uiso 1 1 calc R . .
C12 C 0.0781(3) -0.0958(4) 0.15216(15) 0.0506(8) Uani 1 1 d . . .
H12 H 0.0049 -0.1032 0.1155 0.047(8) Uiso 1 1 calc R . .
C13 C 0.1150(3) 0.0583(3) 0.18055(13) 0.0410(7) Uani 1 1 d . . .
C14 C 0.0354(3) 0.2064(3) 0.14929(14) 0.0444(7) Uani 1 1 d . . .
H14A H -0.0713 0.1828 0.1416 0.056(8) Uiso 1 1 calc R . .
H14B H 0.0459 0.3011 0.1813 0.047(7) Uiso 1 1 calc R . .
C15 C 0.0470(3) 0.3718(3) 0.04376(12) 0.0377(6) Uani 1 1 d . . .
C16 C 0.1157(3) 0.4008(3) -0.02023(13) 0.0392(6) Uani 1 1 d . . .
H16 H 0.1952 0.3332 -0.0339 0.033(6) Uiso 1 1 calc R . .
C17 C 0.0682(3) 0.5285(3) -0.06402(13) 0.0399(7) Uani 1 1 d . . .
H17 H 0.1146 0.5468 -0.1075 0.054(8) 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
C15 O3 C14 116.79(19) . . ?
C5 N1 C1 114.1(6) . . ?
N1 C1 C2 125.8(6) . . ?
C1 C2 C3 119.0(5) . . ?
C2 C3 C4 116.3(3) . . ?
C2 C3 C6 120.4(5) . . ?
C4 C3 C6 123.3(5) . . ?
C5 C4 C3 118.2(4) . . ?
N1 C5 C4 126.5(6) . . ?
C6 C6 C3 127.9(5) 3_676 . ?
C1A N1A C5A 120.0 . . ?
C2A C1A N1A 120.0 . . ?
C1A C2A C3A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C4A C3A C6A 121.6(6) . . ?
C2A C3A C6A 118.4(6) . . ?
C5A C4A C3A 120.0 . . ?
C4A C5A N1A 120.0 . . ?
C6A C6A C3A 126.8(11) 3_676 . ?
O2 C7 O1 123.9(2) . . ?
O2 C7 C8 123.5(2) . . ?
O1 C7 C8 112.6(2) . . ?
C13 C8 C9 119.4(2) . . ?
C13 C8 C7 122.9(2) . . ?
C9 C8 C7 117.7(2) . . ?
C10 C9 C8 121.1(3) . . ?
C11 C10 C9 119.5(3) . . ?
C10 C11 C12 120.1(3) . . ?
C11 C12 C13 121.2(3) . . ?
C8 C13 C12 118.6(2) . . ?
C8 C13 C14 124.0(2) . . ?
C12 C13 C14 117.4(2) . . ?
O3 C14 C13 106.5(2) . . ?
C17 C15 O3 125.1(2) 3_565 . ?
C17 C15 C16 119.7(2) 3_565 . ?
O3 C15 C16 115.3(2) . . ?
C17 C16 C15 120.6(2) . . ?
C15 C17 C16 119.8(2) 3_565 . ?
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 C7 1.311(3) . ?
O2 C7 1.211(3) . ?
O3 C15 1.384(3) . ?
O3 C14 1.437(3) . ?
N1 C5 1.306(5) . ?
N1 C1 1.320(5) . ?
C1 C2 1.358(8) . ?
C2 C3 1.385(7) . ?
C3 C4 1.389(7) . ?
C3 C6 1.457(5) . ?
C4 C5 1.366(7) . ?
C6 C6 1.296(10) 3_676 ?
N1A C1A 1.3900 . ?
N1A C5A 1.3900 . ?
C1A C2A 1.3900 . ?
C2A C3A 1.3900 . ?
C3A C4A 1.3900 . ?
C3A C6A 1.471(9) . ?
C4A C5A 1.3900 . ?
C6A C6A 1.35(2) 3_676 ?
C7 C8 1.500(3) . ?
C8 C13 1.388(4) . ?
C8 C9 1.401(4) . ?
C9 C10 1.374(4) . ?
C10 C11 1.374(5) . ?
C11 C12 1.383(4) . ?
C12 C13 1.396(4) . ?
C13 C14 1.508(4) . ?
C15 C17 1.373(4) 3_565 ?
C15 C16 1.388(4) . ?
C16 C17 1.383(4) . ?
C17 C15 1.373(4) 3_565 ?
