#------------------------------------------------------------------------------
#$Date: 2019-11-23 13:03:14 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233407 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/88/4348824.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_4348824
loop_
_publ_author_name
'Falaise, Clément'
'Delille, Jason'
'Volkringer, Christophe'
'Vezin, Hervé'
'Rabu, Pierre'
'Loiseau, Thierry'
_publ_section_title
;
 Series of Hydrated Heterometallic Uranyl-Cobalt(II) Coordination Polymers
 with Aromatic Polycarboxylate Ligands: Formation of U═O-Co Bonding
 upon Dehydration Process.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10453
_journal_page_last               10466
_journal_paper_doi               10.1021/acs.inorgchem.6b01697
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C24 H12 Co O25 U2'
_chemical_formula_weight         1235.33
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3900(2)
_cell_length_b                   18.0142(3)
_cell_length_c                   21.9051(4)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.478
_cell_measurement_theta_min      2.445
_cell_volume                     3310.72(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            36597
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    10.355
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5409
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.812
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0188
_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/[σ²(Fo²)+(0.0152P)²+0.2179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                4876
_reflns_number_total             5062
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic6b01697_si_004.cif
_cod_data_source_block           jd145-invers
_cod_database_code               4348824
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
O1A O 0.2467(3) 0.92180(12) 0.32474(10) 0.0276(5) Uani 1 1 d .
OW3 O -0.2451(3) 1.06988(11) 0.24114(11) 0.0356(6) Uani 1 1 d .
O2A O 0.3848(3) 0.81951(11) 0.32054(11) 0.0291(5) Uani 1 1 d .
OW2 O -0.0034(4) 1.16781(13) 0.18091(13) 0.0511(7) Uani 1 1 d .
OW1 O -0.0240(4) 1.01004(12) 0.32246(11) 0.0381(6) Uani 1 1 d .
OU2 O 0.6126(3) 0.94471(12) 0.30286(10) 0.0330(6) Uani 1 1 d .
OU1 O 0.4299(3) 0.90227(12) 0.44339(10) 0.0341(6) Uani 1 1 d .
C3A C 0.0000 0.8537(2) 0.2500 0.0217(9) Uani 1 2 d S
H3A H 0.0000 0.9053 0.2500 0.026 Uiso 1 2 calc SR
C2A C 0.1253(4) 0.81539(15) 0.27633(14) 0.0217(6) Uani 1 1 d .
C1A C 0.2581(4) 0.85400(17) 0.30835(14) 0.0228(6) Uani 1 1 d .
C7A C 0.0000 0.7005(2) 0.2500 0.0266(10) Uani 1 2 d S
H7A H 0.0000 0.6489 0.2500 0.032 Uiso 1 2 calc SR
O2B O 0.4039(3) 1.05007(10) 0.37457(13) 0.0319(5) Uani 1 1 d .
C1B C 0.5267(3) 1.07741(15) 0.40017(14) 0.0232(6) Uani 1 1 d .
O1B O 0.6411(3) 1.03506(12) 0.41345(13) 0.0375(6) Uani 1 1 d .
C4B C 0.4219(4) 1.28006(14) 0.41442(13) 0.0206(6) Uani 1 1 d .
C6B C 0.5610(4) 1.30822(16) 0.43933(14) 0.0253(7) Uani 1 1 d .
H6B H 0.5698 1.3588 0.4473 0.030 Uiso 1 1 calc R
C8B C 0.6743(4) 1.18567(17) 0.44018(15) 0.0266(7) Uani 1 1 d .
H8B H 0.7584 1.1539 0.4494 0.032 Uiso 1 1 calc R
C7B C 0.6879(4) 1.26096(18) 0.45239(15) 0.0288(7) Uani 1 1 d .
H7B H 0.7813 1.2798 0.4692 0.035 Uiso 1 1 calc R
O3B O 0.6615(3) 0.80366(11) 0.37672(13) 0.0354(6) Uani 1 1 d .
O4B O 0.7886(3) 0.89841(11) 0.41450(11) 0.0306(5) Uani 1 1 d .
OW4 O -0.0768(5) 1.0000 0.5000 0.0403(9) Uani 1 2 d S
OW5 O 0.0917(4) 1.09637(19) 0.42666(14) 0.0679(9) Uani 1 1 d .
C2B C 0.5373(4) 1.15766(15) 0.41453(13) 0.0213(6) Uani 1 1 d .
C3B C 0.4100(4) 1.20490(15) 0.40107(14) 0.0210(6) Uani 1 1 d .
H3B H 0.3177 1.1861 0.3833 0.025 Uiso 1 1 calc R
C6A C 0.1266(4) 0.73841(16) 0.27590(14) 0.0248(7) Uani 1 1 d .
H6A H 0.2117 0.7125 0.2928 0.030 Uiso 1 1 calc R
C5B C 0.7846(4) 0.82964(15) 0.40114(15) 0.0238(7) Uani 1 1 d .
U1 U 0.519708(12) 0.921694(6) 0.372620(5) 0.01981(3) Uani 1 1 d .
Co2 Co 0.0000 1.08976(3) 0.2500 0.02690(13) Uani 1 2 d S
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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'
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
C1A O1A U1 92.77(18) . .
C1A O2A U1 96.79(18) . .
C2A C3A C2A 120.2(4) 3 .
C3A C2A C6A 120.1(3) . .
C3A C2A C1A 122.1(3) . .
C6A C2A C1A 117.7(3) . .
O2A C1A O1A 118.4(3) . .
O2A C1A C2A 120.1(3) . .
O1A C1A C2A 121.6(3) . .
O2A C1A U1 57.45(15) . .
O1A C1A U1 60.94(16) . .
C2A C1A U1 177.2(2) . .
C6A C7A C6A 120.9(4) . 3
C1B O2B U1 92.92(16) . .
O1B C1B O2B 119.0(2) . .
O1B C1B C2B 119.7(3) . .
O2B C1B C2B 121.3(3) . .
O1B C1B U1 58.16(15) . .
O2B C1B U1 60.81(14) . .
C2B C1B U1 177.7(2) . .
C1B O1B U1 95.95(18) . .
C6B C4B C3B 120.1(3) . .
C6B C4B C5B 120.7(2) . 5_455
C3B C4B C5B 119.2(3) . 5_455
C4B C6B C7B 120.1(3) . .
C2B C8B C7B 120.4(3) . .
C8B C7B C6B 119.7(3) . .
C5B O3B U1 95.29(16) . .
C5B O4B U1 93.19(18) . .
C8B C2B C3B 120.1(3) . .
C8B C2B C1B 119.7(3) . .
C3B C2B C1B 120.2(3) . .
C4B C3B C2B 119.6(3) . .
C7A C6A C2A 119.4(3) . .
O3B C5B O4B 118.9(3) . .
O3B C5B C4B 119.9(2) . 5_545
O4B C5B C4B 121.3(3) . 5_545
O3B C5B U1 58.65(15) . .
O4B C5B U1 60.24(15) . .
C4B C5B U1 178.3(2) 5_545 .
OU1 U1 OU2 177.63(11) . .
OU1 U1 O3B 90.17(10) . .
OU2 U1 O3B 91.22(10) . .
OU1 U1 O2A 93.63(10) . .
OU2 U1 O2A 88.70(10) . .
O3B U1 O2A 65.56(7) . .
OU1 U1 O1B 91.27(10) . .
OU2 U1 O1B 86.37(10) . .
O3B U1 O1B 120.69(8) . .
O2A U1 O1B 172.09(8) . .
OU1 U1 O4B 91.71(10) . .
OU2 U1 O4B 87.60(10) . .
O3B U1 O4B 52.62(7) . .
O2A U1 O4B 117.92(7) . .
O1B U1 O4B 68.07(7) . .
OU1 U1 O2B 90.15(10) . .
OU2 U1 O2B 88.23(10) . .
O3B U1 O2B 172.86(8) . .
O2A U1 O2B 121.54(7) . .
O1B U1 O2B 52.17(7) . .
O4B U1 O2B 120.24(7) . .
OU1 U1 O1A 88.73(10) . .
OU2 U1 O1A 92.34(10) . .
O3B U1 O1A 117.36(7) . .
O2A U1 O1A 52.05(7) . .
O1B U1 O1A 121.95(7) . .
O4B U1 O1A 169.96(7) . .
O2B U1 O1A 69.78(7) . .
OU1 U1 C5B 91.43(10) . .
OU2 U1 C5B 88.97(10) . .
O3B U1 C5B 26.06(7) . .
O2A U1 C5B 91.45(8) . .
O1B U1 C5B 94.64(8) . .
O4B U1 C5B 26.57(7) . .
O2B U1 C5B 146.80(8) . .
O1A U1 C5B 143.40(8) . .
OU1 U1 C1B 91.03(10) . .
OU2 U1 C1B 86.75(10) . .
O3B U1 C1B 146.58(8) . .
O2A U1 C1B 147.57(8) . .
O1B U1 C1B 25.89(7) . .
O4B U1 C1B 93.96(7) . .
O2B U1 C1B 26.28(7) . .
O1A U1 C1B 96.06(7) . .
C5B U1 C1B 120.52(8) . .
OU1 U1 C1A 91.17(10) . .
OU2 U1 C1A 90.73(10) . .
O3B U1 C1A 91.18(8) . .
O2A U1 C1A 25.76(8) . .
O1B U1 C1A 148.03(8) . .
O4B U1 C1A 143.68(8) . .
O2B U1 C1A 95.95(8) . .
O1A U1 C1A 26.29(8) . .
C5B U1 C1A 117.16(9) . .
C1B U1 C1A 122.18(8) . .
OW2 Co2 OW2 94.22(16) 3 .
OW2 Co2 OW3 101.39(11) 3 .
OW2 Co2 OW3 92.01(11) . .
OW2 Co2 OW3 92.01(11) 3 3
OW2 Co2 OW3 101.39(11) . 3
OW3 Co2 OW3 160.32(12) . 3
OW2 Co2 OW1 85.13(10) 3 .
OW2 Co2 OW1 173.79(15) . .
OW3 Co2 OW1 82.09(10) . .
OW3 Co2 OW1 84.80(10) 3 .
OW2 Co2 OW1 173.79(15) 3 3
OW2 Co2 OW1 85.13(10) . 3
OW3 Co2 OW1 84.80(10) . 3
OW3 Co2 OW1 82.09(10) 3 3
OW1 Co2 OW1 96.18(13) . 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1A C1A 1.277(4) .
O1A U1 2.519(2) .
OW3 Co2 2.096(2) .
O2A C1A 1.260(4) .
O2A U1 2.443(2) .
OW2 Co2 2.066(2) .
OW1 Co2 2.150(2) .
OU2 U1 1.765(2) .
OU1 U1 1.759(2) .
C3A C2A 1.384(3) 3
C3A C2A 1.384(3) .
C2A C6A 1.387(4) .
C2A C1A 1.489(4) .
C1A U1 2.879(3) .
C7A C6A 1.385(4) .
C7A C6A 1.385(4) 3
O2B C1B 1.272(3) .
O2B U1 2.5086(19) .
C1B O1B 1.260(3) .
C1B C2B 1.482(4) .
C1B U1 2.870(3) .
O1B U1 2.451(2) .
C4B C6B 1.385(4) .
C4B C3B 1.389(4) .
C4B C5B 1.486(4) 5_455
C6B C7B 1.393(4) .
C8B C2B 1.375(4) .
C8B C7B 1.387(4) .
O3B C5B 1.254(4) .
O3B U1 2.4381(19) .
O4B C5B 1.273(3) .
O4B U1 2.472(2) .
C2B C3B 1.398(4) .
C5B C4B 1.486(4) 5_545
C5B U1 2.843(3) .
Co2 OW2 2.066(2) 3
Co2 OW3 2.096(2) 3
Co2 OW1 2.150(2) 3
