#------------------------------------------------------------------------------
#$Date: 2017-03-06 01:51:07 +0200 (Mon, 06 Mar 2017) $
#$Revision: 193985 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/55/4345506.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_4345506
loop_
_publ_author_name
'Li, Zhi'
'Pierri, Agustin E.'
'Huang, Po-Ju'
'Wu, Guang'
'Iretskii, Alexei V.'
'Ford, Peter C.'
_publ_section_title
;
 Dinuclear PhotoCORMs: Dioxygen-Assisted Carbon Monoxide Uncaging from
 Long-Wavelength-Absorbing Metal--Metal-Bonded Carbonyl Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b03138
_journal_year                    2017
_chemical_formula_sum            'C21.5 H9 Ce Cl Mn N2 O9'
_chemical_formula_weight         669.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                111.712(8)
_cell_angle_beta                 90.526(8)
_cell_angle_gamma                114.312(8)
_cell_formula_units_Z            2
_cell_length_a                   9.888(3)
_cell_length_b                   10.582(3)
_cell_length_c                   12.887(4)
_cell_measurement_reflns_used    922
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1120.7(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8923
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.467
_diffrn_reflns_theta_min         1.733
_exptl_absorpt_coefficient_mu    2.745
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.620
_refine_diff_density_min         -2.563
_refine_diff_density_rms         0.262
_refine_ls_extinction_coef       0.0223(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5413
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0739P)²+16.4591P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4599
_reflns_number_total             5413
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b03138_si_005.cif
_cod_data_source_block           05052016_0m
_cod_original_cell_volume        1120.8(6)
_cod_original_formula_sum        'C21.50 H9 Ce Cl Mn N2 O9'
_cod_database_code               4345506
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.875
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8362(11) 0.0342(11) 0.9685(8) 0.0333(19) Uani 1 1 d . . . . .
C2 C 0.7886(12) -0.1806(11) 0.7735(8) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.5770(10) -0.1097(10) 0.8478(8) 0.0326(19) Uani 1 1 d . . . . .
C4 C 0.7756(13) -0.2011(12) 0.5392(9) 0.044(2) Uani 1 1 d . . . . .
C5 C 0.4972(12) -0.3401(11) 0.6041(9) 0.038(2) Uani 1 1 d . . . . .
C6 C 0.4648(13) -0.0770(12) 0.6504(9) 0.042(2) Uani 1 1 d . . . . .
C7 C 0.7331(13) 0.0528(13) 0.5847(9) 0.044(2) Uani 1 1 d . . . . .
C8 C 0.4990(12) -0.2413(12) 0.4259(9) 0.042(2) Uani 1 1 d . . . . .
C9 C 0.6332(10) 0.2201(11) 0.8998(7) 0.0321(19) Uani 1 1 d . . . . .
H9 H 0.5479 0.1444 0.9107 0.039 Uiso 1 1 calc R U . . .
C10 C 0.6370(11) 0.3596(11) 0.9243(8) 0.0328(19) Uani 1 1 d . . . . .
H10 H 0.5539 0.3766 0.9501 0.039 Uiso 1 1 calc R U . . .
C11 C 0.7590(11) 0.4758(11) 0.9123(7) 0.0307(18) Uani 1 1 d . . . . .
C12 C 0.8817(11) 0.4475(11) 0.8735(7) 0.0320(19) Uani 1 1 d . . . . .
C13 C 1.0155(11) 0.5559(11) 0.8568(8) 0.035(2) Uani 1 1 d . . . . .
H13 H 1.0244 0.6536 0.8695 0.042 Uiso 1 1 calc R U . . .
C14 C 1.1309(11) 0.5201(11) 0.8226(8) 0.035(2) Uani 1 1 d . . . . .
H14 H 1.2194 0.5938 0.8129 0.043 Uiso 1 1 calc R U . . .
C15 C 1.1194(11) 0.3712(10) 0.8009(7) 0.0317(19) Uani 1 1 d . . . . .
C16 C 1.2373(11) 0.3330(12) 0.7685(9) 0.038(2) Uani 1 1 d . . . . .
H16 H 1.3293 0.4043 0.7604 0.046 Uiso 1 1 calc R U . . .
C17 C 1.2142(12) 0.1864(12) 0.7486(9) 0.037(2) Uani 1 1 d . . . . .
H17 H 1.2913 0.1561 0.7264 0.044 Uiso 1 1 calc R U . . .
C18 C 1.0760(11) 0.0823(12) 0.7615(8) 0.037(2) Uani 1 1 d . . . . .
H18 H 1.0625 -0.0173 0.7472 0.044 Uiso 1 1 calc R U . . .
C19 C 0.9852(10) 0.2624(10) 0.8134(8) 0.0305(18) Uani 1 1 d . . . . .
C20 C 0.8691(10) 0.3014(10) 0.8508(7) 0.0300(18) Uani 1 1 d . . . . .
C21 C 0.7626(13) 0.6263(12) 0.9432(8) 0.040(2) Uani 1 1 d . . . . .
H21 H 0.8560 0.7102 0.9520 0.048 Uiso 1 1 calc R U . . .
Ce1 Ce 0.60731(4) -0.15063(4) 0.58171(3) 0.01478(17) Uani 1 1 d . . . . .
C22 C 1.044(2) 0.5053(17) 0.4319(12) 0.056(6) Uiso 0.5 1 d D . P A 1
Cl1 Cl 0.8873(7) 0.3241(7) 0.3769(5) 0.0534(14) Uiso 0.5 1 d D . P A 1
Cl2 Cl 0.9109(9) 0.4220(10) 0.4182(7) 0.074(2) Uiso 0.5 1 d . . P B 2
Mn2 Mn 0.76342(16) -0.00870(15) 0.82506(11) 0.0299(3) Uani 1 1 d . . . . .
N1 N 0.7458(9) 0.1864(9) 0.8609(6) 0.0308(16) Uani 1 1 d . . . . .
N2 N 0.9639(9) 0.1185(9) 0.7928(6) 0.0325(16) Uani 1 1 d . . . . .
O1 O 0.8745(9) 0.0519(9) 1.0597(6) 0.0467(18) Uani 1 1 d . . . . .
O2 O 0.8038(10) -0.2893(9) 0.7451(7) 0.0497(19) Uani 1 1 d . . . . .
O3 O 0.4617(9) -0.1711(9) 0.8680(7) 0.0490(19) Uani 1 1 d . . . . .
O4 O 0.8776(10) -0.2272(12) 0.5164(7) 0.061(2) Uani 1 1 d . . . . .
O5 O 0.4343(10) -0.4467(9) 0.6200(7) 0.053(2) Uani 1 1 d . . . . .
O6 O 0.3792(11) -0.0320(10) 0.6911(7) 0.056(2) Uani 1 1 d . . . . .
O7 O 0.8084(10) 0.1709(9) 0.5851(7) 0.055(2) Uani 1 1 d . . . . .
O8 O 0.4360(9) -0.2967(9) 0.3355(6) 0.0463(18) Uani 1 1 d . . . . .
O9 O 0.6501(11) 0.6475(11) 0.9578(8) 0.060(2) 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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_3
O1 C1 Mn2 175.1(9) .
O2 C2 Mn2 177.3(9) .
O3 C3 Mn2 176.5(9) .
O4 C4 Ce1 178.2(10) .
O5 C5 Ce1 178.2(9) .
O6 C6 Ce1 179.4(10) .
O7 C7 Ce1 178.7(11) .
O8 C8 Ce1 178.5(9) .
N1 C9 C10 122.7(9) .
C9 C10 C11 121.6(9) .
C10 C11 C12 118.1(9) .
C10 C11 C21 120.5(9) .
C12 C11 C21 121.4(9) .
C20 C12 C11 116.7(9) .
C20 C12 C13 118.7(9) .
C11 C12 C13 124.7(9) .
C14 C13 C12 120.6(9) .
C13 C14 C15 120.9(9) .
C16 C15 C19 119.5(9) .
C16 C15 C14 121.9(9) .
C19 C15 C14 118.5(9) .
C17 C16 C15 117.4(9) .
C16 C17 C18 120.1(9) .
N2 C18 C17 122.6(9) .
N2 C19 C20 117.6(9) .
N2 C19 C15 122.3(9) .
C20 C19 C15 120.1(9) .
N1 C20 C19 114.3(8) .
N1 C20 C12 124.5(9) .
C19 C20 C12 121.2(9) .
O9 C21 C11 122.8(10) .
C8 Ce1 C6 95.4(4) .
C8 Ce1 C4 94.7(5) .
C6 Ce1 C4 169.7(4) .
C8 Ce1 C7 95.9(4) .
C6 Ce1 C7 88.8(5) .
C4 Ce1 C7 87.8(5) .
C8 Ce1 C5 93.1(4) .
C6 Ce1 C5 90.0(5) .
C4 Ce1 C5 91.8(5) .
C7 Ce1 C5 171.0(4) .
C8 Ce1 Mn2 177.7(3) .
C6 Ce1 Mn2 82.3(3) .
C4 Ce1 Mn2 87.6(3) .
C7 Ce1 Mn2 84.4(3) .
C5 Ce1 Mn2 86.6(3) .
Cl1 C22 C22 76.9(8) 2_766
C1 Mn2 C3 88.2(4) .
C1 Mn2 C2 90.5(4) .
C3 Mn2 C2 91.0(5) .
C1 Mn2 N1 96.4(4) .
C3 Mn2 N1 94.6(4) .
C2 Mn2 N1 171.3(4) .
C1 Mn2 N2 96.0(4) .
C3 Mn2 N2 173.3(4) .
C2 Mn2 N2 94.2(4) .
N1 Mn2 N2 79.8(3) .
C1 Mn2 Ce1 167.4(3) .
C3 Mn2 Ce1 83.8(3) .
C2 Mn2 Ce1 80.0(3) .
N1 Mn2 Ce1 94.0(2) .
N2 Mn2 Ce1 93.0(2) .
C9 N1 C20 116.4(8) .
C9 N1 Mn2 128.3(7) .
C20 N1 Mn2 115.1(6) .
C18 N2 C19 118.0(9) .
C18 N2 Mn2 128.7(7) .
C19 N2 Mn2 113.2(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.153(12) .
C1 Mn2 1.797(9) .
C2 O2 1.145(12) .
C2 Mn2 1.815(10) .
C3 O3 1.145(12) .
C3 Mn2 1.801(9) .
C4 O4 1.164(14) .
C4 Ce1 1.972(12) .
C5 O5 1.138(13) .
C5 Ce1 1.982(11) .
C6 O6 1.172(14) .
C6 Ce1 1.948(12) .
C7 O7 1.160(14) .
C7 Ce1 1.979(12) .
C8 O8 1.127(13) .
C8 Ce1 1.946(11) .
C9 N1 1.351(12) .
C9 C10 1.374(14) .
C10 C11 1.384(14) .
C11 C12 1.418(13) .
C11 C21 1.477(14) .
C12 C20 1.413(13) .
C12 C13 1.432(14) .
C13 C14 1.372(14) .
C14 C15 1.449(14) .
C15 C16 1.404(14) .
C15 C19 1.412(13) .
C16 C17 1.392(15) .
C17 C18 1.418(14) .
C18 N2 1.335(13) .
C19 N2 1.367(12) .
C19 C20 1.405(13) .
C20 N1 1.372(12) .
C21 O9 1.225(13) .
Ce1 Mn2 2.9985(16) .
C22 Cl1 1.762(9) .
C22 C22 1.98(4) 2_766
Cl2 Cl2 2.288(17) 2_766
Mn2 N1 2.024(8) .
Mn2 N2 2.036(9) .
