#------------------------------------------------------------------------------
#$Date: 2019-11-19 04:58:33 +0200 (Tue, 19 Nov 2019) $
#$Revision: 231022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/19/7701971.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_7701971
loop_
_publ_author_name
'Wang, Xue-Zhi'
'Sun, Meng-Ying'
'Zheng, Ji'
'Luo, Dong'
'Li, Qi'
'Zhou, Xiao-Ping'
'Li, Dan'
_publ_section_title
;
 Coordination-Driven Self-Assembly of M10L8 Metal-Organic Bi-capped Square
 Antiprisms with Adaptable Cavity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04368C
_journal_year                    2019
_chemical_formula_moiety         '0.5(C44 H50 Cu4 N24), Cl O4'
_chemical_formula_sum            'C22 H25 Cl Cu2 N12 O4'
_chemical_formula_weight         684.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc20ncgj
_audit_creation_date             2019-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-06 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4211(5)
_cell_length_b                   14.8334(5)
_cell_length_c                   21.6671(10)
_cell_measurement_reflns_used    4309
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.4800
_cell_measurement_theta_min      5.5440
_cell_volume                     3027.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  32.00   0.50    1.50    --    0.00  38.00   0.00   96
  2  ω     54.00  89.00   0.50    1.50    --    0.00  38.00  90.00   70
  3  ω    -17.00  50.00   0.50    1.50    --    0.00  38.00  90.00  134
  4  ω     55.00  80.00   0.50    1.50    --    0.00  38.00   0.00   50
  5  ω     29.00 120.00   0.50    6.00    --   89.30 -82.00 -90.00  182
  6  ω     78.00 179.00   0.50    6.00    --   89.30  30.00 120.00  202
  7  ω    113.00 169.00   0.50    6.00    --   89.30  61.00  30.00  112
  8  ω     66.00 105.00   0.50    6.00    --   89.30  61.00  30.00   78
  9  ω     50.00 102.00   0.50    6.00    --   89.30 -82.00-150.00  104
 10  ω     66.00 143.00   0.50    6.00    --   89.30  61.00  60.00  154
 11  ω      5.00 113.00   0.50    6.00    --   89.30 -61.00 -90.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1043711000
_diffrn_orient_matrix_UB_12      0.0413773000
_diffrn_orient_matrix_UB_13      0.0467894000
_diffrn_orient_matrix_UB_21      0.1225223000
_diffrn_orient_matrix_UB_22      0.0142426000
_diffrn_orient_matrix_UB_23      0.0460866000
_diffrn_orient_matrix_UB_31      0.0273893000
_diffrn_orient_matrix_UB_32      0.0942591000
_diffrn_orient_matrix_UB_33      -0.0274211000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.109
_diffrn_reflns_theta_min         4.081
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       plank
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0660
_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)+(0.0984P)²+4.8361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2302
_reflns_number_total             2886
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04368c2.cif
_cod_data_source_block           CP5
_cod_database_code               7701971
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O H Cu Cl'
_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_max   0.943
_shelx_estimated_absorpt_t_min   0.756
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Fixed Sof: H1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C11(H11), C10(H10), C1(H1A), C4(H4), C8(H8), C2(H2)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.850
_oxdiff_exptl_absorpt_empirical_full_min 0.342
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, 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
Cu1 Cu 0.31764(7) 0.60765(4) 0.51101(3) 0.0273(3) Uani 1 1 d . . .
Cl1 Cl 0.500000 0.82045(11) 0.750000 0.0575(6) Uani 1 2 d S T P
N5 N 0.4732(4) 0.6968(2) 0.49256(16) 0.0270(8) Uani 1 1 d . . .
N6 N 0.6429(4) 0.8003(2) 0.47493(16) 0.0271(8) Uani 1 1 d . . .
N3 N 0.2311(4) 0.4809(2) 0.51601(17) 0.0299(8) Uani 1 1 d . . .
N2 N 0.3646(4) 0.5802(2) 0.59863(17) 0.0289(8) Uani 1 1 d . . .
N4 N 0.3052(4) 0.6051(2) 0.41835(19) 0.0326(9) Uani 1 1 d . . .
N1 N 0.4398(4) 0.5516(2) 0.69433(17) 0.0348(9) Uani 1 1 d . . .
H1 H 0.479523 0.559401 0.730701 0.042 Uiso 0.5 1 calc R . .
C11 C 0.5713(5) 0.7519(3) 0.5175(2) 0.0286(10) Uani 1 1 d . . .
H11 H 0.588432 0.756122 0.560579 0.034 Uiso 1 1 calc R . .
C3 C 0.3247(5) 0.4932(3) 0.6145(2) 0.0301(10) Uani 1 1 d . . .
C9 C 0.4833(5) 0.7125(3) 0.4298(2) 0.0300(9) Uani 1 1 d . . .
C10 C 0.5873(5) 0.7753(3) 0.4198(2) 0.0296(9) Uani 1 1 d . . .
H10 H 0.615933 0.797639 0.380589 0.036 Uiso 1 1 calc R . .
C1 C 0.4327(5) 0.6126(3) 0.6473(2) 0.0313(10) Uani 1 1 d . . .
H1A H 0.472101 0.671467 0.649178 0.038 Uiso 1 1 calc R . .
C4 C 0.2529(5) 0.4427(3) 0.5682(2) 0.0344(10) Uani 1 1 d . . .
H4 H 0.222148 0.382671 0.575687 0.041 Uiso 1 1 calc R . .
C8 C 0.3914(5) 0.6593(3) 0.3907(2) 0.0327(10) Uani 1 1 d . . .
H8 H 0.394374 0.663926 0.346953 0.039 Uiso 1 1 calc R . .
C5 C 0.1563(5) 0.4328(3) 0.4670(2) 0.0337(10) Uani 1 1 d . . .
H5A H 0.056187 0.453058 0.465910 0.040 Uiso 1 1 calc R . .
H5B H 0.156771 0.367434 0.476260 0.040 Uiso 1 1 calc R . .
C2 C 0.3721(6) 0.4757(3) 0.6733(2) 0.0354(11) Uani 1 1 d . . .
H2 H 0.360201 0.420888 0.695341 0.042 Uiso 1 1 calc R . .
C7 C 0.2116(6) 0.5469(3) 0.3821(2) 0.0386(11) Uani 1 1 d . . .
H7A H 0.238838 0.549885 0.338000 0.046 Uiso 1 1 calc R . .
H7B H 0.112387 0.568259 0.385883 0.046 Uiso 1 1 calc R . .
C6 C 0.2219(6) 0.4479(3) 0.4050(2) 0.0404(12) Uani 1 1 d . . .
H6A H 0.174728 0.408110 0.374638 0.049 Uiso 1 1 calc R . .
H6B H 0.323198 0.430366 0.406938 0.049 Uiso 1 1 calc R . .
O1 O 0.5801(7) 0.8708(6) 0.7892(4) 0.153(4) Uani 1 1 d . . .
O2 O 0.5948(6) 0.7676(5) 0.7171(4) 0.156(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 0.0181 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N5 Cu1 N6 99.64(14) . 4_466
N5 Cu1 N3 154.32(15) . .
N3 Cu1 N6 105.59(15) . 4_466
N2 Cu1 N5 99.31(15) . .
N2 Cu1 N6 99.45(14) . 4_466
N2 Cu1 N3 81.41(15) . .
N2 Cu1 N4 163.86(15) . .
N4 Cu1 N5 81.78(14) . .
N4 Cu1 N6 96.21(14) . 4_466
N4 Cu1 N3 90.69(15) . .
O1 Cl1 O1 113.4(9) 3_656 .
O1 Cl1 O2 110.3(6) 3_656 .
O1 Cl1 O2 105.9(4) 3_656 3_656
O1 Cl1 O2 105.9(4) . .
O1 Cl1 O2 110.3(6) . 3_656
O2 Cl1 O2 111.0(8) . 3_656
C11 N5 Cu1 144.9(3) . .
C11 N5 C9 104.2(4) . .
C9 N5 Cu1 110.8(3) . .
C11 N6 Cu1 128.4(3) . 4_566
C11 N6 C10 105.3(4) . .
C10 N6 Cu1 126.2(3) . 4_566
C4 N3 Cu1 112.8(3) . .
C4 N3 C5 120.2(4) . .
C5 N3 Cu1 126.9(3) . .
C3 N2 Cu1 111.5(3) . .
C1 N2 Cu1 142.4(3) . .
C1 N2 C3 105.7(4) . .
C8 N4 Cu1 114.5(3) . .
C8 N4 C7 119.8(4) . .
C7 N4 Cu1 125.6(3) . .
C1 N1 H1 127.1 . .
C1 N1 C2 105.8(4) . .
C2 N1 H1 127.1 . .
N5 C11 N6 113.1(4) . .
N5 C11 H11 123.4 . .
N6 C11 H11 123.4 . .
N2 C3 C4 116.3(4) . .
C2 C3 N2 108.6(4) . .
C2 C3 C4 135.1(4) . .
N5 C9 C8 116.3(4) . .
C10 C9 N5 108.7(4) . .
C10 C9 C8 135.0(4) . .
N6 C10 C9 108.8(4) . .
N6 C10 H10 125.6 . .
C9 C10 H10 125.6 . .
N2 C1 N1 112.2(4) . .
N2 C1 H1A 123.9 . .
N1 C1 H1A 123.9 . .
N3 C4 C3 117.7(4) . .
N3 C4 H4 121.1 . .
C3 C4 H4 121.1 . .
N4 C8 C9 116.4(4) . .
N4 C8 H8 121.8 . .
C9 C8 H8 121.8 . .
N3 C5 H5A 109.1 . .
N3 C5 H5B 109.1 . .
N3 C5 C6 112.3(4) . .
H5A C5 H5B 107.9 . .
C6 C5 H5A 109.1 . .
C6 C5 H5B 109.1 . .
N1 C2 C3 107.7(4) . .
N1 C2 H2 126.2 . .
C3 C2 H2 126.2 . .
N4 C7 H7A 109.6 . .
N4 C7 H7B 109.6 . .
N4 C7 C6 110.3(4) . .
H7A C7 H7B 108.1 . .
C6 C7 H7A 109.6 . .
C6 C7 H7B 109.6 . .
C5 C6 C7 113.8(4) . .
C5 C6 H6A 108.8 . .
C5 C6 H6B 108.8 . .
C7 C6 H6A 108.8 . .
C7 C6 H6B 108.8 . .
H6A C6 H6B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N5 2.014(4) .
Cu1 N6 2.160(4) 4_466
Cu1 N3 2.053(4) .
Cu1 N2 1.991(4) .
Cu1 N4 2.011(4) .
Cl1 O1 1.360(6) .
Cl1 O1 1.360(5) 3_656
Cl1 O2 1.386(6) .
Cl1 O2 1.386(6) 3_656
N5 C11 1.346(5) .
N5 C9 1.383(5) .
N6 C11 1.349(5) .
N6 C10 1.357(6) .
N3 C4 1.281(6) .
N3 C5 1.461(6) .
N2 C3 1.387(5) .
N2 C1 1.324(6) .
N4 C8 1.291(6) .
N4 C7 1.463(6) .
N1 H1 0.8800 .
N1 C1 1.365(5) .
N1 C2 1.372(6) .
C11 H11 0.9500 .
C3 C4 1.425(6) .
C3 C2 1.373(6) .
C9 C10 1.369(6) .
C9 C8 1.446(6) .
C10 H10 0.9500 .
C1 H1A 0.9500 .
C4 H4 0.9500 .
C8 H8 0.9500 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C5 C6 1.494(7) .
C2 H2 0.9500 .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C7 C6 1.553(6) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.356 0.250 95 39 ' '
2 0.000 0.644 0.750 94 39 ' '
3 0.500 0.144 0.750 94 39 ' '
4 0.500 0.856 0.250 95 39 ' '
