#------------------------------------------------------------------------------
#$Date: 2016-08-07 12:35:16 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185606 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/55/7055585.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_7055585
loop_
_publ_author_name
'Dai, Fangna'
'Fan, Weidong'
'Bi, Jiahui'
'Zhang, Qian'
'Zhang, XiRui'
'Liang, Tuo'
'Wang, Xingyi'
'Dong, Bin'
'Gao, Jing'
_publ_section_title
;
 Four Pb(ii) metal--organic frameworks with increasing dimensions:
 structural diversities by varying the ligands
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              6867
_journal_paper_doi               10.1039/C5NJ03632A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         '0.25(C80 H48 O16 Pb4)'
_chemical_formula_sum            'C20 H12 O4 Pb'
_chemical_formula_weight         523.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_space_group_name_Hall  '-I 2yc'
_symmetry_space_group_name_H-M   'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-24 deposited with the CCDC.
2016-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.458(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7028(3)
_cell_length_b                   5.3856(2)
_cell_length_c                   35.9661(15)
_cell_measurement_reflns_used    3146
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.2230
_cell_measurement_theta_min      3.4100
_cell_volume                     1485.26(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 16.0450
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details
;
  1 omega   31.00   61.00   1.0000    2.1100
omega____ theta____ kappa____ phi______ frames
    -       18.9813  -99.0000   30.0000 30

  2 omega   36.00   97.00   1.0000    2.1100
omega____ theta____ kappa____ phi______ frames
    -       18.9813  178.0000    0.0000 61

  3 omega    8.00   92.00   1.0000    2.1100
omega____ theta____ kappa____ phi______ frames
    -       18.9813   38.0000   60.0000 84

  4 omega  -51.00    2.00   1.0000    2.1100
omega____ theta____ kappa____ phi______ frames
    -       18.9813  -38.0000   60.0000 53

  5 omega   35.00   74.00   1.0000    2.1100
omega____ theta____ kappa____ phi______ frames
    -       18.9813  178.0000 -120.0000 39

  6 omega  -13.00   90.00   1.0000    2.1100
omega____ theta____ kappa____ phi______ frames
    -       18.9813   77.0000 -180.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0260120000
_diffrn_orient_matrix_UB_12      -0.1263340000
_diffrn_orient_matrix_UB_13      0.0007438000
_diffrn_orient_matrix_UB_21      -0.0310786000
_diffrn_orient_matrix_UB_22      -0.0141357000
_diffrn_orient_matrix_UB_23      -0.0190970000
_diffrn_orient_matrix_UB_31      0.0831411000
_diffrn_orient_matrix_UB_32      0.0342612000
_diffrn_orient_matrix_UB_33      -0.0052592000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            5131
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.918
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.341
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0268
_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)+(0.0166P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1676
_reflns_number_total             1742
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5nj03632a2.cif
_cod_data_source_block           643
_cod_depositor_comments
'Adding full bibliography for 7055584--7055587.cif.'
_cod_original_cell_volume        1485.25(10)
_cod_database_code               7055585
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N Co'
_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.
;
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C11(H11), C12(H12), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb -0.5000 0.43180(4) 0.2500 0.01776(9) Uani 1 2 d S T P
O1 O -0.2189(5) 0.4205(5) 0.21803(10) 0.0279(8) Uani 1 1 d . . .
O2 O -0.0779(6) 0.7621(7) 0.20369(11) 0.0529(12) Uani 1 1 d . . .
C2 C -0.3559(5) 0.5096(7) 0.07789(12) 0.0138(8) Uani 1 1 d . . .
C3 C -0.4285(6) 0.5020(7) 0.03814(12) 0.0140(9) Uani 1 1 d . . .
C5 C -0.1732(7) 0.5771(8) 0.19499(14) 0.0234(11) Uani 1 1 d . . .
C6 C -0.3302(6) 0.3402(8) 0.14094(13) 0.0206(10) Uani 1 1 d . . .
H6 H -0.3553 0.2141 0.1573 0.025 Uiso 1 1 calc R . .
C7 C -0.1902(6) 0.7243(7) 0.12916(13) 0.0194(9) Uani 1 1 d . . .
H7 H -0.1204 0.8581 0.1373 0.023 Uiso 1 1 calc R . .
C9 C -0.2517(6) 0.7077(7) 0.09202(13) 0.0195(9) Uani 1 1 d . . .
H9 H -0.2231 0.8323 0.0758 0.023 Uiso 1 1 calc R . .
C11 C -0.5374(6) 0.3131(8) 0.02382(13) 0.0219(10) Uani 1 1 d . . .
H11 H -0.5645 0.1841 0.0395 0.026 Uiso 1 1 calc R . .
C12 C -0.3936(6) 0.6888(8) 0.01284(13) 0.0230(10) Uani 1 1 d . . .
H12 H -0.3210 0.8193 0.0212 0.028 Uiso 1 1 calc R . .
C14 C -0.3912(6) 0.3236(7) 0.10376(13) 0.0189(9) Uani 1 1 d . . .
H14 H -0.4573 0.1864 0.0955 0.023 Uiso 1 1 calc R . .
C15 C -0.2308(6) 0.5445(7) 0.15452(13) 0.0163(9) 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'
Pb Pb -3.3944 10.1111 '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
O1 Pb1 O1 177.26(13) 2_455 .
O1 Pb1 O1 108.17(11) 2_455 7_455
O1 Pb1 O1 108.17(11) . 8_455
O1 Pb1 O1 91.52(14) 8_455 7_455
O1 Pb1 O1 69.80(12) . 7_455
O1 Pb1 O1 69.80(12) 2_455 8_455
O2 Pb1 O1 152.15(13) 8_465 7_455
O2 Pb1 O1 82.48(13) 7_465 2_455
O2 Pb1 O1 99.45(13) 7_465 .
O2 Pb1 O1 99.44(13) 8_465 2_455
O2 Pb1 O1 94.73(13) 7_465 7_455
O2 Pb1 O1 94.73(13) 8_465 8_455
O2 Pb1 O1 152.15(13) 7_465 8_455
O2 Pb1 O1 82.47(13) 8_465 .
O2 Pb1 O2 92.3(2) 7_465 8_465
Pb1 O1 Pb1 110.20(12) . 7_455
C5 O1 Pb1 123.1(3) . 7_455
C5 O1 Pb1 125.8(3) . .
C5 O2 Pb1 145.5(4) . 7_465
C9 C2 C3 121.3(4) . .
C9 C2 C14 116.2(4) . .
C14 C2 C3 122.5(4) . .
C11 C3 C2 122.5(4) . .
C11 C3 C12 115.6(4) . .
C12 C3 C2 121.9(4) . .
O1 C5 O2 124.1(5) . .
O1 C5 C15 119.3(4) . .
O2 C5 C15 116.6(4) . .
C14 C6 C15 120.9(4) . .
C9 C7 C15 121.0(4) . .
C7 C9 C2 122.2(4) . .
C12 C11 C3 121.8(4) 5_465 .
C11 C12 C3 122.6(4) 5_465 .
C6 C14 C2 121.7(4) . .
C6 C15 C5 122.3(4) . .
C7 C15 C5 119.7(4) . .
C7 C15 C6 118.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.547(4) 2_455
Pb1 O1 2.719(3) 7_455
Pb1 O1 2.719(3) 8_455
Pb1 O1 2.547(4) .
Pb1 O2 2.379(4) 8_465
Pb1 O2 2.379(4) 7_465
O1 Pb1 2.719(3) 7_455
O1 C5 1.256(6) .
O2 Pb1 2.379(4) 7_465
O2 C5 1.260(5) .
C2 C3 1.485(6) .
C2 C9 1.401(6) .
C2 C14 1.411(6) .
C3 C11 1.387(6) .
C3 C12 1.400(6) .
C5 C15 1.491(7) .
C6 C14 1.377(6) .
C6 C15 1.401(6) .
C7 C9 1.377(6) .
C7 C15 1.386(6) .
C11 C12 1.374(6) 5_465
C12 C11 1.374(6) 5_465
