#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/19/7011927.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_7011927
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            'C22 H18 O6'
_chemical_formula_weight         378.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.1050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1936(2)
_cell_length_b                   7.24040(10)
_cell_length_c                   17.31980(10)
_cell_measurement_reflns_used    5866
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     1894.51(4)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9897
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.9610
_exptl_absorpt_correction_T_min  0.5604
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'rectangular shape, cut'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0129(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0443
_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/[σ²(Fo²)+(0.0675P)²+0.2356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                2779
_reflns_number_total             3765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205942h.txt
_cod_data_source_block           diacid1
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7011927
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.49483(10) 0.81455(19) 0.44279(8) 0.0738(4) Uani 1 1 d . . .
O2 O 0.56912(11) 1.0753(2) 0.43035(9) 0.0750(5) Uani 1 1 d . . .
H2 H 0.5458(12) 1.102(3) 0.4703(11) 0.050 Uiso 1 1 d . . .
O3 O 0.47043(10) 0.40295(18) 0.27759(8) 0.0712(4) Uani 1 1 d . . .
O4 O 0.45437(8) 0.14893(15) 0.17678(7) 0.0517(3) Uani 1 1 d . . .
O5 O 0.49194(10) -0.30171(19) 0.03899(9) 0.0753(5) Uani 1 1 d . . .
O6 O 0.38554(11) -0.4379(2) -0.03738(11) 0.0905(6) Uani 1 1 d . . .
H6 H 0.4284(13) -0.520(3) -0.0385(10) 0.050 Uiso 1 1 d . . .
C1 C 0.54351(12) 0.9116(2) 0.40700(11) 0.0536(4) Uani 1 1 d . . .
C2 C 0.57783(11) 0.8489(2) 0.33431(10) 0.0493(4) Uani 1 1 d . . .
C3 C 0.63774(14) 0.9614(3) 0.30121(12) 0.0622(5) Uani 1 1 d . . .
H3 H 0.6530(14) 1.073(3) 0.3254(12) 0.070(6) Uiso 1 1 d . . .
C4 C 0.67407(14) 0.9087(3) 0.23473(12) 0.0678(5) Uani 1 1 d . . .
H4 H 0.7167(17) 0.987(3) 0.2140(13) 0.086(7) Uiso 1 1 d . . .
C5 C 0.64954(13) 0.7416(3) 0.20044(12) 0.0635(5) Uani 1 1 d . . .
H5 H 0.6735(14) 0.703(3) 0.1521(12) 0.072(6) Uiso 1 1 d . . .
C6 C 0.58966(12) 0.6286(3) 0.23186(10) 0.0553(5) Uani 1 1 d . . .
H6A H 0.5701(15) 0.509(3) 0.2083(13) 0.077(6) Uiso 1 1 d . . .
C7 C 0.55178(11) 0.6784(2) 0.29899(9) 0.0475(4) Uani 1 1 d . . .
C8 C 0.48455(13) 0.5537(2) 0.33020(11) 0.0533(4) Uani 1 1 d . . .
H8A H 0.4268(13) 0.619(3) 0.3330(11) 0.058(5) Uiso 1 1 d . . .
H8B H 0.5061(13) 0.508(3) 0.3822(12) 0.064(6) Uiso 1 1 d . . .
C9 C 0.41193(12) 0.2679(2) 0.29289(10) 0.0498(4) Uani 1 1 d . . .
C10 C 0.36390(14) 0.2601(3) 0.35621(11) 0.0604(5) Uani 1 1 d . . .
H10 H 0.3716(13) 0.357(3) 0.3934(12) 0.066(6) Uiso 1 1 d . . .
C11 C 0.30660(15) 0.1140(3) 0.36423(12) 0.0681(5) Uani 1 1 d . . .
H11 H 0.2711(16) 0.109(3) 0.4081(14) 0.084(7) Uiso 1 1 d . . .
C12 C 0.29775(15) -0.0226(3) 0.30950(13) 0.0710(6) Uani 1 1 d . . .
H12 H 0.2585(16) -0.121(3) 0.3132(13) 0.085(7) Uiso 1 1 d . . .
C13 C 0.34573(13) -0.0168(3) 0.24547(11) 0.0591(5) Uani 1 1 d . . .
H13 H 0.3399(14) -0.113(3) 0.2081(13) 0.075(6) Uiso 1 1 d . . .
C14 C 0.40331(11) 0.1266(2) 0.23721(9) 0.0456(4) Uani 1 1 d . . .
C15 C 0.45550(12) 0.0005(3) 0.12207(10) 0.0502(4) Uani 1 1 d . . .
H15A H 0.4610(12) -0.115(3) 0.1489(11) 0.057(5) Uiso 1 1 d . . .
H15B H 0.5125(14) 0.020(3) 0.0982(11) 0.063(5) Uiso 1 1 d . . .
C16 C 0.37573(11) 0.0044(2) 0.06125(9) 0.0453(4) Uani 1 1 d . . .
C17 C 0.31908(13) 0.1554(3) 0.05697(11) 0.0581(5) Uani 1 1 d . . .
H17 H 0.3322(12) 0.257(3) 0.0938(11) 0.058(5) Uiso 1 1 d . . .
C18 C 0.24460(15) 0.1623(3) 0.00373(13) 0.0722(6) Uani 1 1 d . . .
H18 H 0.2072(15) 0.262(3) 0.0040(13) 0.079(7) Uiso 1 1 d . . .
C19 C 0.22464(15) 0.0177(3) -0.04654(13) 0.0715(6) Uani 1 1 d . . .
H19 H 0.1720(18) 0.019(4) -0.0816(15) 0.103(8) Uiso 1 1 d . . .
C20 C 0.28024(13) -0.1325(3) -0.04485(11) 0.0597(5) Uani 1 1 d . . .
H20 H 0.2679(14) -0.234(3) -0.0794(12) 0.071(6) Uiso 1 1 d . . .
C21 C 0.35599(11) -0.1414(2) 0.00824(9) 0.0464(4) Uani 1 1 d . . .
C22 C 0.41696(12) -0.3004(2) 0.00540(10) 0.0509(4) Uani 1 1 d . . .
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'
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
C9 O3 C8 118.79(14) . . ?
C14 O4 C15 117.48(13) . . ?
O1 C1 O2 122.62(17) . . ?
O1 C1 C2 122.36(15) . . ?
O2 C1 C2 115.02(17) . . ?
C3 C2 C7 119.89(16) . . ?
C3 C2 C1 118.37(16) . . ?
C7 C2 C1 121.75(16) . . ?
C4 C3 C2 121.24(19) . . ?
C5 C4 C3 119.1(2) . . ?
C6 C5 C4 120.62(18) . . ?
C5 C6 C7 121.55(18) . . ?
C6 C7 C2 117.58(17) . . ?
C6 C7 C8 119.95(15) . . ?
C2 C7 C8 122.47(15) . . ?
O3 C8 C7 106.96(14) . . ?
O3 C9 C10 126.35(15) . . ?
O3 C9 C14 113.83(15) . . ?
C10 C9 C14 119.82(16) . . ?
C9 C10 C11 120.06(18) . . ?
C12 C11 C10 119.96(19) . . ?
C11 C12 C13 120.65(19) . . ?
C14 C13 C12 119.94(18) . . ?
C13 C14 O4 125.74(15) . . ?
C13 C14 C9 119.56(16) . . ?
O4 C14 C9 114.69(14) . . ?
O4 C15 C16 112.32(14) . . ?
C17 C16 C21 117.84(16) . . ?
C17 C16 C15 119.71(15) . . ?
C21 C16 C15 122.44(14) . . ?
C18 C17 C16 121.53(18) . . ?
C19 C18 C17 120.29(19) . . ?
C18 C19 C20 119.7(2) . . ?
C19 C20 C21 120.81(18) . . ?
C20 C21 C16 119.84(16) . . ?
C20 C21 C22 119.25(15) . . ?
C16 C21 C22 120.84(15) . . ?
O5 C22 O6 122.11(16) . . ?
O5 C22 C21 123.00(15) . . ?
O6 C22 C21 114.87(16) . . ?
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 C1 1.234(2) . ?
O2 C1 1.298(2) . ?
O3 C9 1.366(2) . ?
O3 C8 1.4235(19) . ?
O4 C14 1.377(2) . ?
O4 C15 1.4340(19) . ?
O5 C22 1.223(2) . ?
O6 C22 1.301(2) . ?
C1 C2 1.484(2) . ?
C2 C3 1.390(3) . ?
C2 C7 1.416(2) . ?
C3 C4 1.383(3) . ?
C4 C5 1.381(3) . ?
C5 C6 1.378(3) . ?
C6 C7 1.398(2) . ?
C7 C8 1.506(3) . ?
C9 C10 1.382(3) . ?
C9 C14 1.403(2) . ?
C10 C11 1.386(3) . ?
C11 C12 1.367(3) . ?
C12 C13 1.391(3) . ?
C13 C14 1.375(2) . ?
C15 C16 1.519(2) . ?
C16 C17 1.389(2) . ?
C16 C21 1.410(2) . ?
C17 C18 1.383(3) . ?
C18 C19 1.375(3) . ?
C19 C20 1.375(3) . ?
C20 C21 1.396(3) . ?
C21 C22 1.481(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21146611
