#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:45:22 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180052 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/46/7034684.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_7034684
loop_
_publ_author_name
'Chen, Di-Ming'
'Ma, Jian-Gong'
'Cheng, Peng'
_publ_section_title
;
 Solvent-induced secondary building unit (SBU) variations in a series of
 Cu(ii) metal-organic frameworks derived from a bifunctional ligand.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8926
_journal_page_last               8931
_journal_paper_doi               10.1039/c5dt00994d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '0.25(C216 H152 Cl28 Cu32 N72 O72)'
_chemical_formula_sum            'C54 H38 Cl7 Cu8 N18 O18'
_chemical_formula_weight         1983.49
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-03-05 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8022(7)
_cell_length_b                   24.0290(12)
_cell_length_c                   21.3108(8)
_cell_measurement_temperature    293(2)
_cell_volume                     8091.9(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10178
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.361
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3932
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3676
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0595P)²+31.6573P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                3225
_reflns_number_total             3676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00994d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7034682--7034684.cif.'
_cod_database_code               7034684
#BEGIN Tags that were not found in dictionaries:
_olex2_refinement_description
;
1. Others
 Fixed Sof: C2(0.5) C8(0.5) C9(0.5) H9(0.5) C3(0.5) H3(0.5) O6(0.5) C4(0.5)
 C5(0.5) H5(0.5) C13(0.5) H13(0.5) O0AA(0.5)
 Fixed U13: Cu1(0) Cu2(0) Cl4(0) O2(0) N5(0) Cl1(0) O1(0) O4(0)
 Fixed U23: Cu1(0) Cu2(0) Cl4(0) O2(0) N5(0) Cl1(0) O1(0) O4(0)
 Fixed Uiso: H17(0.039) H31(0.043) H10(0.036) H11(0.033) H15(0.068) H16(0.063)
 H1(0.06) H9(0.034) H3(0.036) H5(0.036) H13(0.037)
 Fixed X: H17(0.1661) H31(0.3453) H10(0.3082) H11(0.2463) H15(0.0965)
 H16(0.036) H1(0.5764) Cl1(0.25) H9(0.7057) H3(0.8414) H5(0.6916) H13(0.8276)
 Fixed Y: H17(0.0917) H31(0.1681) H10(0.057) H11(0.0218) H15(0.1424)
 H16(0.1089) H1(0.2828) Cl1(0.25) H9(0.2915) H3(0.3264) H5(0.3536) H13(0.3904)
 Fixed Z: Cu1(0.5) Cu2(0.5) Cl4(0.5) O2(0.5) H17(0.6225) H31(0.7167)
 H10(0.7761) H11(0.8663) H15(0.7385) H16(0.8298) H1(0.5915) N5(0.5) Cl1(0.5)
 O1(0.5) H9(0.3917) H3(0.3815) O4(0.5) H5(0.4339) H13(0.445) H2(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z'
3 'x, -y, -z+1/2'
4 '-x, y, -z+1/2'
5 'x+1/2, y+1/2, z'
6 '-x+1/2, -y+1/2, z'
7 'x+1/2, -y+1/2, -z+1/2'
8 '-x+1/2, y+1/2, -z+1/2'
9 '-x, -y, -z'
10 'x, y, -z'
11 '-x, y, z-1/2'
12 'x, -y, z-1/2'
13 '-x+1/2, -y+1/2, -z'
14 'x+1/2, y+1/2, -z'
15 '-x+1/2, y+1/2, z-1/2'
16 'x+1/2, -y+1/2, z-1/2'
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_calc_flag
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.05001(4) 0.04399(3) 0.5000 0.01728(17) Uani 1 d 2 S T P
Cu2 Cu 0.25872(4) 0.14218(3) 0.5000 0.01809(18) Uani 1 d 2 S T P
Cu3 Cu 0.40677(3) 0.20975(2) 0.57925(2) 0.03072(17) Uani 1 d 1 . . .
Cl4 Cl 0.11491(7) 0.13375(5) 0.5000 0.0192(3) Uani 1 d 2 S T P
O2 O 0.3822(2) 0.16586(16) 0.5000 0.0207(8) Uani 1 d 2 DS T P
N7 N 0.26153(19) 0.13809(14) 0.59180(14) 0.0246(7) Uani 1 d 1 . . .
N9 N 0.3234(2) 0.16535(16) 0.62457(15) 0.0291(8) Uani 1 d 1 . . .
N10 N 0.2432(2) 0.12172(17) 0.69080(15) 0.0316(8) Uani 1 d 1 . . .
C17 C 0.2136(3) 0.1128(2) 0.63234(18) 0.0323(10) Uani 1 d 1 . . .
H17 H 0.1661 0.0917 0.6225 0.039 Uiso 1 calc 1 R . .
C31 C 0.3117(3) 0.1549(2) 0.68405(19) 0.0357(11) Uani 1 d 1 . . .
H31 H 0.3453 0.1681 0.7167 0.043 Uiso 1 calc 1 R . .
C7 C 0.2068(3) 0.10126(19) 0.74865(18) 0.0312(10) Uani 1 d 1 . . .
C10 C 0.2530(3) 0.06650(19) 0.78655(18) 0.0299(9) Uani 1 d 1 . . .
H10 H 0.3082 0.0570 0.7761 0.036 Uiso 1 calc 1 R . .
C11 C 0.2162(3) 0.04593(17) 0.84044(18) 0.0271(9) Uani 1 d 1 . . .
H11 H 0.2463 0.0218 0.8663 0.033 Uiso 1 calc 1 R . .
C12 C 0.1344(2) 0.06116(17) 0.85612(17) 0.0244(8) Uani 1 d 1 . . .
C15 C 0.1262(3) 0.1180(3) 0.7642(2) 0.0566(16) Uani 1 d 1 . . .
H15 H 0.0965 0.1424 0.7385 0.068 Uiso 1 calc 1 R . .
C16 C 0.0903(3) 0.0978(3) 0.8185(2) 0.0525(15) Uani 1 d 1 . . .
H16 H 0.0360 0.1089 0.8298 0.063 Uiso 1 calc 1 R . .
C6 C 0.0918(2) 0.03810(17) 0.91296(17) 0.0241(8) Uani 1 d 1 . . .
O3 O 0.11860(18) -0.00684(12) 0.93525(13) 0.0310(7) Uani 1 d 1 . . .
O5 O 0.02976(18) 0.06547(12) 0.93381(13) 0.0340(7) Uani 1 d 1 . . .
N3 N 0.4935(2) 0.24993(14) 0.53182(16) 0.0294(7) Uani 1 d 1 . . .
C1 C 0.5610(3) 0.27657(19) 0.5499(3) 0.0497(15) Uani 1 d 1 . . .
H1 H 0.5764 0.2828 0.5915 0.060 Uiso 1 calc 1 R . .
N5 N 0.6049(3) 0.2936(2) 0.5000 0.054(2) Uani 1 d 2 S T P
Cl2 Cl 0.42380(11) 0.26706(6) 0.66317(6) 0.0656(5) Uani 1 d 1 . . .
Cl1 Cl 0.2500 0.2500 0.5000 0.0656(9) Uani 1 d 4 S T P
O1 O 0.2922(3) 0.0418(2) 0.5000 0.0607(15) Uani 1 d 2 S T P
C2 C 0.6882(5) 0.3193(3) 0.4802(3) 0.0176(16) Uani 0.50 d 1 . . .
C8 C 0.8478(6) 0.3616(4) 0.4668(4) 0.0274(19) Uani 0.50 d 1 . . .
C9 C 0.7309(5) 0.3110(4) 0.4245(4) 0.0281(18) Uani 0.50 d 1 . . .
H9 H 0.7057 0.2915 0.3917 0.034 Uiso 0.50 calc 1 R . .
C3 C 0.8114(5) 0.3321(4) 0.4184(4) 0.0298(18) Uani 0.50 d 1 . . .
H3 H 0.8414 0.3264 0.3815 0.036 Uiso 0.50 calc 1 R . .
O4 O 0.9751(3) 0.4012(2) 0.5000 0.0483(13) Uani 1 d 2 S T P
O6 O 0.9797(4) 0.3678(3) 0.4110(4) 0.0381(16) Uani 0.50 d 1 . . .
C4 C 0.9412(5) 0.3786(4) 0.4618(4) 0.033(2) Uani 0.50 d 1 . . .
C5 C 0.7220(5) 0.3484(4) 0.4708(4) 0.0303(19) Uani 0.50 d 1 . . .
H5 H 0.6916 0.3536 0.4339 0.036 Uiso 0.50 calc 1 R . .
C13 C 0.8032(6) 0.3702(4) 0.4776(4) 0.030(2) Uani 0.50 d 1 . . .
H13 H 0.8276 0.3904 0.4450 0.037 Uiso 0.50 calc 1 R . .
O0AA O 0.9864(5) 0.3515(3) 0.3752(4) 0.0493(19) Uani 0.50 d 1 . . .
H2 H 0.415(5) 0.138(2) 0.5000 0.08(3) Uiso 1 d 2 DS T P
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 '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
Cl4 Cu1 Cu1 168.64(5) . 9_556
O3 Cu1 Cu1 88.08(8) 3_556 9_556
O3 Cu1 Cu1 88.08(8) 12 9_556
O3 Cu1 Cl4 99.97(8) 12 .
O3 Cu1 Cl4 99.97(8) 3_556 .
O3 Cu1 O3 89.00(18) 3_556 12
O5 Cu1 Cu1 79.98(8) 11 9_556
O5 Cu1 Cu1 79.98(8) 4_556 9_556
O5 Cu1 Cl4 92.19(9) 11 .
O5 Cu1 Cl4 92.19(9) 4_556 .
O5 Cu1 O3 167.82(12) 11 3_556
O5 Cu1 O3 167.82(12) 4_556 12
O5 Cu1 O3 88.23(13) 11 12
O5 Cu1 O3 88.23(13) 4_556 3_556
O5 Cu1 O5 92.00(19) 11 4_556
Cl4 Cu2 Cl1 92.05(4) . .
Cl4 Cu2 O1 97.27(13) . .
O2 Cu2 Cl4 168.84(12) . .
O2 Cu2 Cl1 76.79(11) . .
O2 Cu2 O1 93.89(17) . .
N7 Cu2 Cl4 91.04(9) 10_556 .
N7 Cu2 Cl4 91.04(9) . .
N7 Cu2 O2 89.56(9) 10_556 .
N7 Cu2 O2 89.56(9) . .
N7 Cu2 N7 173.7(2) 10_556 .
N7 Cu2 Cl1 92.95(10) . .
N7 Cu2 Cl1 92.95(10) 10_556 .
N7 Cu2 O1 86.91(10) 10_556 .
N7 Cu2 O1 86.91(10) . .
O1 Cu2 Cl1 170.68(12) . .
O2 Cu3 Cl2 173.03(12) . .
N9 Cu3 O2 89.93(13) . .
N9 Cu3 N3 176.41(16) . .
N9 Cu3 Cl2 91.25(11) . .
N3 Cu3 O2 87.72(13) . .
N3 Cu3 Cl2 91.41(11) . .
Cu2 Cl4 Cu1 120.52(6) . .
Cu3 O2 Cu2 109.21(12) 10_556 .
Cu3 O2 Cu2 109.21(12) . .
Cu3 O2 Cu3 112.73(17) 10_556 .
N9 N7 Cu2 120.1(2) . .
C17 N7 Cu2 132.4(3) . .
C17 N7 N9 107.5(3) . .
N7 N9 Cu3 119.4(2) . .
C31 N9 Cu3 133.0(3) . .
C31 N9 N7 107.6(3) . .
C17 N10 C31 105.9(3) . .
C17 N10 C7 126.6(3) . .
C31 N10 C7 127.5(3) . .
N7 C17 N10 109.7(3) . .
N9 C31 N10 109.3(3) . .
C10 C7 N10 119.8(4) . .
C10 C7 C15 121.9(4) . .
C15 C7 N10 118.3(4) . .
C7 C10 C11 118.9(4) . .
C10 C11 C12 120.0(4) . .
C11 C12 C6 121.3(3) . .
C16 C12 C11 120.0(4) . .
C16 C12 C6 118.7(4) . .
C7 C15 C16 118.7(4) . .
C15 C16 C12 120.3(4) . .
O3 C6 C12 118.3(3) . .
O3 C6 O5 125.3(3) . .
O5 C6 C12 116.3(3) . .
C6 O3 Cu1 118.0(2) . 3_556
C6 O5 Cu1 128.0(3) . 11_556
N3 N3 Cu3 121.09(10) 10_556 .
C1 N3 Cu3 131.5(4) . .
C1 N3 N3 107.2(3) . 10_556
N3 C1 N5 109.9(5) . .
C1 N5 C1 105.8(5) 10_556 .
C1 N5 C2 110.7(3) 10_556 .
C1 N5 C2 110.7(3) . 10_556
C1 N5 C2 143.1(4) . .
C1 N5 C2 143.1(4) 10_556 10_556
C2 N5 C2 32.4(5) 10_556 .
Cu2 Cl1 Cu2 180.0 . 13_556
C9 C2 N5 127.3(6) . .
C5 C2 N5 109.6(5) 10_556 .
C5 C2 C9 122.7(7) 10_556 .
C3 C8 C4 119.1(8) . .
C3 C8 C13 120.1(7) . 10_556
C13 C8 C4 120.4(8) 10_556 .
C3 C9 C2 118.6(7) . .
C9 C3 C8 120.4(8) . .
C4 O4 C4 93.7(9) . 10_556
O4 C4 C8 122.7(8) . .
O4 C4 O6 119.4(8) . .
O6 C4 C8 117.8(8) . .
C2 C5 C13 118.3(7) 10_556 .
C8 C13 C5 78.2(6) 10_556 10_556
C5 C13 C8 119.9(8) . 10_556
C5 C13 C5 44.4(7) . 10_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu1 2.6394(12) 9_556
Cu1 Cl4 2.3884(13) .
Cu1 O3 1.969(3) 3_556
Cu1 O3 1.969(3) 12
Cu1 O5 1.961(3) 4_556
Cu1 O5 1.961(3) 11
Cu2 Cl4 2.2815(13) .
Cu2 O2 2.033(3) .
Cu2 N7 1.959(3) .
Cu2 N7 1.959(3) 10_556
Cu2 Cl1 2.5944(7) .
Cu2 O1 2.470(5) .
Cu3 O2 2.029(2) .
Cu3 N9 1.951(3) .
Cu3 N3 1.957(3) .
Cu3 Cl2 2.2732(13) .
O2 Cu3 2.028(2) 10_556
N7 N9 1.368(4) .
N7 C17 1.300(5) .
N9 C31 1.305(5) .
N10 C17 1.348(5) .
N10 C31 1.352(5) .
N10 C7 1.447(5) .
C7 C10 1.373(6) .
C7 C15 1.375(6) .
C10 C11 1.379(6) .
C11 C12 1.384(6) .
C12 C16 1.381(6) .
C12 C6 1.493(5) .
C15 C16 1.377(6) .
C6 O3 1.253(5) .
C6 O5 1.261(5) .
O3 Cu1 1.969(3) 3_556
O5 Cu1 1.961(3) 11_556
N3 N3 1.356(7) 10_556
N3 C1 1.303(5) .
C1 N5 1.334(6) .
N5 C1 1.334(6) 10_556
N5 C2 1.515(9) .
N5 C2 1.515(9) 10_556
Cl1 Cu2 2.5944(7) 13_556
C2 C9 1.380(10) .
C2 C5 1.366(10) 10_556
C8 C3 1.377(12) .
C8 C4 1.534(12) .
C8 C13 1.395(11) 10_556
C9 C3 1.376(11) .
O4 C4 1.116(9) .
O4 C4 1.116(9) 10_556
O6 C4 1.269(12) .
C5 C2 1.366(10) 10_556
C5 C13 1.393(13) .
C13 C8 1.395(11) 10_556
C13 C5 1.769(13) 10_556
O0AA Cu3 2.441(8) 13_656
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 0.500 0.250 238 45 ' '
2 0.000 0.000 0.250 22 2 ' '
3 0.000 0.500 0.750 238 45 ' '
4 0.000 0.000 0.750 22 2 ' '
5 0.250 0.250 0.212 41 13 ' '
6 0.250 0.750 0.288 42 13 ' '
7 0.250 0.750 0.712 41 13 ' '
8 0.250 0.250 0.788 42 13 ' '
9 0.500 1.000 0.250 238 45 ' '
10 0.500 0.000 0.750 238 45 ' '
11 0.500 0.500 0.250 22 2 ' '
12 0.500 0.500 0.750 22 2 ' '
13 0.750 0.750 0.212 41 13 ' '
14 0.750 0.250 0.288 42 13 ' '
15 0.750 0.250 0.712 41 13 ' '
16 0.750 0.750 0.788 42 13 ' '
