#------------------------------------------------------------------------------
#$Date: 2016-10-08 01:15:51 +0300 (Sat, 08 Oct 2016) $
#$Revision: 187112 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/01/7040121.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_7040121
loop_
_publ_author_name
'Zhao, Dan'
'Liu, Xiao-Hui'
'Shi, Zhuang-Zhi'
'Zhu, Chen-Dan'
'Zhao, Yue'
'Wang, Peng'
'Sun, Wei-Yin'
_publ_section_title
;
 Three powerful dinuclear metal-organic catalysts for converting CO2 into
 organic carbonates.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14184
_journal_page_last               14190
_journal_paper_doi               10.1039/c6dt02755e
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration .ad
_chemical_formula_moiety         'C9 H8 O3'
_chemical_formula_sum            'C9 H8 O3'
_chemical_formula_weight         164.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-01 deposited with the CCDC.
2016-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1207(5)
_cell_length_b                   7.5850(6)
_cell_length_c                   16.9844(14)
_cell_measurement_reflns_used    3701
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      5.21
_cell_volume                     788.51(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2920
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        65.494
_diffrn_reflns_theta_max         65.494
_diffrn_reflns_theta_min         6.391
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.230
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.4789
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 469 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(7)
_refine_ls_extinction_coef       0.041(3)
_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   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0255
_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)+(0.0341P)²+0.1194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.597
_reflns_Friedel_fraction_full    0.894
_reflns_Friedel_fraction_max     0.894
_reflns_number_gt                1266
_reflns_number_total             1281
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02755e2.cif
_cod_data_source_block           R
_cod_depositor_comments
'Adding full bibliography for 7040117--7040122.cif.'
_cod_database_code               7040121
_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   0.792
_shelx_estimated_absorpt_t_max   0.824
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.1731(3) 0.6229(2) 0.81908(10) 0.0240(4) Uani 1 1 d . .
C2 C 0.3663(3) 0.7139(2) 0.80671(10) 0.0280(4) Uani 1 1 d . .
H2 H 0.4398 0.7668 0.8499 0.034 Uiso 1 1 calc R U
C3 C 0.1508(3) 0.5624(2) 0.68024(10) 0.0333(5) Uani 1 1 d . .
H3 H 0.0768 0.5108 0.6368 0.040 Uiso 1 1 calc R U
C4 C 0.0644(3) 0.5474(2) 0.75557(10) 0.0284(4) Uani 1 1 d . .
H4 H -0.0687 0.4856 0.7637 0.034 Uiso 1 1 calc R U
C5 C 0.4532(3) 0.7282(2) 0.73135(11) 0.0346(5) Uani 1 1 d . .
H5 H 0.5865 0.7897 0.7231 0.042 Uiso 1 1 calc R U
C6 C 0.3447(4) 0.6525(2) 0.66838(11) 0.0361(5) Uani 1 1 d . .
H6 H 0.4036 0.6623 0.6168 0.043 Uiso 1 1 calc R U
C7 C 0.0905(3) 0.6000(2) 0.90174(10) 0.0251(4) Uani 1 1 d . .
H7 H 0.1713 0.6812 0.9379 0.030 Uiso 1 1 calc R U
C8 C 0.1024(3) 0.4126(2) 0.93328(10) 0.0293(4) Uani 1 1 d . .
H8A H 0.1013 0.3255 0.8899 0.035 Uiso 1 1 calc R U
H8B H 0.2352 0.3949 0.9656 0.035 Uiso 1 1 calc R U
C9 C -0.2334(3) 0.5246(2) 0.95841(11) 0.0282(5) Uani 1 1 d . .
O1 O -0.0932(2) 0.39903(17) 0.98069(7) 0.0329(4) Uani 1 1 d . .
O2 O -0.4167(2) 0.5367(2) 0.98225(8) 0.0398(4) Uani 1 1 d . .
O3 O -0.1435(2) 0.63585(16) 0.90660(7) 0.0302(3) 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 0.0181 0.0091 '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 0.0492 0.0322 '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
C2 C1 C4 119.72(16)
C2 C1 C7 119.12(15)
C4 C1 C7 121.09(15)
C1 C2 C5 120.33(17)
C1 C2 H2 119.8
C5 C2 H2 119.8
C6 C3 C4 120.05(17)
C6 C3 H3 120.0
C4 C3 H3 120.0
C3 C4 C1 119.92(17)
C3 C4 H4 120.0
C1 C4 H4 120.0
C6 C5 C2 119.73(18)
C6 C5 H5 120.1
C2 C5 H5 120.1
C3 C6 C5 120.25(17)
C3 C6 H6 119.9
C5 C6 H6 119.9
O3 C7 C1 111.19(14)
O3 C7 C8 101.60(14)
C1 C7 C8 114.91(14)
O3 C7 H7 109.6
C1 C7 H7 109.6
C8 C7 H7 109.6
O1 C8 C7 102.89(14)
O1 C8 H8A 111.2
C7 C8 H8A 111.2
O1 C8 H8B 111.2
C7 C8 H8B 111.2
H8A C8 H8B 109.1
O2 C9 O1 124.11(18)
O2 C9 O3 124.08(19)
O1 C9 O3 111.81(15)
C9 O1 C8 108.84(13)
C9 O3 C7 108.87(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.385(3)
C1 C4 1.391(2)
C1 C7 1.502(2)
C2 C5 1.390(3)
C2 H2 0.9500
C3 C6 1.384(3)
C3 C4 1.389(3)
C3 H3 0.9500
C4 H4 0.9500
C5 C6 1.383(3)
C5 H5 0.9500
C6 H6 0.9500
C7 O3 1.460(2)
C7 C8 1.521(2)
C7 H7 1.0000
C8 O1 1.446(2)
C8 H8A 0.9900
C8 H8B 0.9900
C9 O2 1.196(2)
C9 O1 1.337(2)
C9 O3 1.338(2)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C4 C1 C2 C5 -0.8(3)
C7 C1 C2 C5 176.21(16)
C6 C3 C4 C1 0.0(3)
C2 C1 C4 C3 0.5(3)
C7 C1 C4 C3 -176.45(16)
C1 C2 C5 C6 0.6(3)
C4 C3 C6 C5 -0.1(3)
C2 C5 C6 C3 -0.2(3)
C2 C1 C7 O3 135.15(16)
C4 C1 C7 O3 -47.9(2)
C2 C1 C7 C8 -110.16(18)
C4 C1 C7 C8 66.8(2)
O3 C7 C8 O1 -23.62(16)
C1 C7 C8 O1 -143.76(15)
O2 C9 O1 C8 173.21(18)
O3 C9 O1 C8 -7.2(2)
C7 C8 O1 C9 19.72(18)
O2 C9 O3 C7 170.10(17)
O1 C9 O3 C7 -9.48(19)
C1 C7 O3 C9 143.50(14)
C8 C7 O3 C9 20.77(17)
