#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/07/7220763.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_7220763
loop_
_publ_author_name
'Huang, Yong-Qing'
'Cheng, Hai-Di'
'Chen, Huai-Ying'
'Wan, Yi'
'Liu, Cheng-Long'
'Zhao, Yue'
'Xiao, Xin-Feng'
'Chen, Li-Hui'
_publ_section_title
;
 Structural diversity in coordination polymers with a semirigid Lewis
 acidity ligand: structures and properties
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5690
_journal_paper_doi               10.1039/C5CE00677E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C32 H50 Cl2 Cu4 N4 O30'
_chemical_formula_sum            'C32 H50 Cl2 Cu4 N4 O30'
_chemical_formula_weight         1295.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-06-18 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.697(6)
_cell_length_b                   25.050(17)
_cell_length_c                   11.638(8)
_cell_measurement_reflns_used    6992
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.43
_cell_volume                     2460(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16373
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  0.7246
_exptl_absorpt_correction_T_min  0.7009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs(Bruker, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0378
_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)+(0.0678P)²+1.8143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                4759
_reflns_number_total             5654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00677e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7220763--7220767.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7220763
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.58793(4) 0.033192(12) 0.60365(2) 0.02581(10) Uani 1 1 d .
Cu2 Cu 0.27507(4) 0.084852(12) 0.40521(3) 0.02484(10) Uani 1 1 d .
Cl1 Cl 0.75889(11) 0.10140(4) 0.60414(8) 0.0498(2) Uani 1 1 d .
O1 O 0.3567(2) 0.05262(9) 0.66777(17) 0.0354(5) Uani 1 1 d .
O2 O 0.1848(2) 0.03370(8) 0.49698(15) 0.0311(4) Uani 1 1 d .
O3 O 0.3407(3) -0.02152(9) 1.22751(16) 0.0385(5) Uani 1 1 d .
O4 O 0.1808(3) 0.04856(10) 1.22133(17) 0.0438(6) Uani 1 1 d .
O5 O 0.5755(2) 0.37437(9) -0.12476(18) 0.0363(5) Uani 1 1 d .
O6 O 0.6664(3) 0.33427(11) 0.0491(2) 0.0526(6) Uani 1 1 d .
O7 O 0.3624(3) 0.14424(9) 0.3320(2) 0.0457(6) Uani 1 1 d .
O8 O 0.5650(3) 0.10552(10) 0.2763(2) 0.0486(6) Uani 1 1 d .
O9 O 0.4742(2) 0.04340(7) 0.43822(14) 0.0237(4) Uani 1 1 d .
H99A H 0.5455 0.0567 0.3912 0.028 Uiso 1 1 calc R
N1 N 0.1588(3) 0.01098(10) 0.79894(19) 0.0310(5) Uani 1 1 d .
N2 N 0.4283(3) 0.26219(9) 0.0093(2) 0.0333(5) Uani 1 1 d .
C1 C 0.0971(4) 0.05014(14) 0.8518(3) 0.0393(7) Uani 1 1 d .
H1A H 0.0321 0.0756 0.8059 0.047 Uiso 1 1 calc R
C2 C 0.1290(4) 0.05315(13) 0.9736(2) 0.0366(6) Uani 1 1 d .
H2A H 0.0864 0.0807 1.0098 0.044 Uiso 1 1 calc R
C3 C 0.2247(3) 0.01499(11) 1.0416(2) 0.0266(5) Uani 1 1 d .
C4 C 0.2909(4) -0.02409(13) 0.9846(3) 0.0391(7) Uani 1 1 d .
H4A H 0.3589 -0.0494 1.0283 0.047 Uiso 1 1 calc R
C5 C 0.2558(4) -0.02532(14) 0.8626(3) 0.0416(7) Uani 1 1 d .
H5A H 0.3000 -0.0517 0.8243 0.050 Uiso 1 1 calc R
C6 C 0.1143(4) 0.00653(15) 0.6678(2) 0.0383(7) Uani 1 1 d .
H6A H 0.0101 0.0221 0.6380 0.046 Uiso 1 1 calc R
H6B H 0.1076 -0.0309 0.6460 0.046 Uiso 1 1 calc R
C7 C 0.2315(3) 0.03409(11) 0.6090(2) 0.0248(5) Uani 1 1 d .
C8 C 0.2506(3) 0.01485(12) 1.1761(2) 0.0279(5) Uani 1 1 d .
C9 C 0.3242(4) 0.26132(14) 0.0775(4) 0.0484(9) Uani 1 1 d .
H9A H 0.2444 0.2869 0.0668 0.058 Uiso 1 1 calc R
C10 C 0.3348(4) 0.22277(13) 0.1633(4) 0.0494(9) Uani 1 1 d .
H10A H 0.2633 0.2226 0.2112 0.059 Uiso 1 1 calc R
C11 C 0.4520(3) 0.18431(11) 0.1782(3) 0.0316(6) Uani 1 1 d .
C12 C 0.5575(4) 0.18577(13) 0.1059(3) 0.0394(7) Uani 1 1 d .
H12A H 0.6371 0.1603 0.1140 0.047 Uiso 1 1 calc R
C13 C 0.5426(4) 0.22544(13) 0.0221(3) 0.0416(7) Uani 1 1 d .
H13A H 0.6133 0.2267 -0.0263 0.050 Uiso 1 1 calc R
C14 C 0.4214(4) 0.30504(12) -0.0787(3) 0.0377(7) Uani 1 1 d .
H14A H 0.3274 0.3266 -0.0832 0.045 Uiso 1 1 calc R
H14B H 0.4141 0.2894 -0.1561 0.045 Uiso 1 1 calc R
C15 C 0.5688(3) 0.34056(11) -0.0451(3) 0.0319(6) Uani 1 1 d .
C16 C 0.4632(4) 0.14025(11) 0.2700(3) 0.0337(6) Uani 1 1 d .
O1W O 0.5505(5) -0.11575(16) 1.1305(3) 0.0932(12) Uani 1 1 d .
O2W O 0.6973(5) 0.31288(19) 0.3020(3) 0.1062(14) Uani 1 1 d .
O3W O 0.9356(5) 0.1510(2) 0.1255(4) 0.1203(17) Uani 1 1 d .
O4W O 0.6762(10) 0.1700(3) -0.1952(7) 0.191(3) Uani 1 1 d .
O5W O 0.4594(7) 0.2265(3) -0.3675(9) 0.216(4) Uani 1 1 d .
O6W O -0.0518(11) 0.1870(6) 0.9100(8) 0.293(7) 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'
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'
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'
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
O3 Cu1 O9 168.77(9) 3_657 .
O3 Cu1 O9 95.90(8) 3_657 3_656
O9 Cu1 O9 81.08(8) . 3_656
O3 Cu1 Cl1 93.57(8) 3_657 .
O9 Cu1 Cl1 94.54(6) . .
O9 Cu1 Cl1 148.68(6) 3_656 .
O3 Cu1 O1 78.38(9) 3_657 .
O9 Cu1 O1 91.01(8) . .
O9 Cu1 O1 94.21(8) 3_656 .
Cl1 Cu1 O1 116.95(7) . .
O3 Cu1 Cu1 134.72(8) 3_657 3_656
O9 Cu1 Cu1 41.33(6) . 3_656
O9 Cu1 Cu1 39.75(5) 3_656 3_656
Cl1 Cu1 Cu1 128.48(4) . 3_656
O1 Cu1 Cu1 93.47(6) . 3_656
O2 Cu2 O7 171.08(9) . .
O2 Cu2 O5 89.04(10) . 4_566
O7 Cu2 O5 86.95(10) . 4_566
O2 Cu2 O9 89.91(9) . .
O7 Cu2 O9 94.01(9) . .
O5 Cu2 O9 178.84(8) 4_566 .
O2 Cu2 O4 98.66(10) . 1_554
O7 Cu2 O4 89.06(11) . 1_554
O5 Cu2 O4 86.54(8) 4_566 1_554
O9 Cu2 O4 94.11(8) . 1_554
C7 O1 Cu1 117.04(17) . .
C7 O2 Cu2 119.11(18) . .
C8 O3 Cu1 127.15(18) . 3_657
C8 O4 Cu2 124.82(18) . 1_556
C15 O5 Cu2 114.29(19) . 4_665
C16 O7 Cu2 125.66(19) . .
Cu1 O9 Cu2 118.07(9) . .
Cu1 O9 Cu1 98.92(8) . 3_656
Cu2 O9 Cu1 106.35(9) . 3_656
Cu1 O9 H99A 110.9 . .
Cu2 O9 H99A 110.9 . .
Cu1 O9 H99A 110.9 3_656 .
C5 N1 C1 120.9(2) . .
C5 N1 C6 119.4(3) . .
C1 N1 C6 119.6(3) . .
C13 N2 C9 120.9(3) . .
C13 N2 C14 118.9(3) . .
C9 N2 C14 120.2(3) . .
N1 C1 C2 120.6(3) . .
N1 C1 H1A 119.7 . .
C2 C1 H1A 119.7 . .
C1 C2 C3 119.6(3) . .
C1 C2 H2A 120.2 . .
C3 C2 H2A 120.2 . .
C2 C3 C4 118.5(2) . .
C2 C3 C8 120.5(2) . .
C4 C3 C8 121.0(2) . .
C5 C4 C3 119.7(3) . .
C5 C4 H4A 120.1 . .
C3 C4 H4A 120.1 . .
N1 C5 C4 120.6(3) . .
N1 C5 H5A 119.7 . .
C4 C5 H5A 119.7 . .
N1 C6 C7 113.0(2) . .
N1 C6 H6A 109.0 . .
C7 C6 H6A 109.0 . .
N1 C6 H6B 109.0 . .
C7 C6 H6B 109.0 . .
H6A C6 H6B 107.8 . .
O1 C7 O2 126.6(2) . .
O1 C7 C6 121.4(2) . .
O2 C7 C6 112.0(2) . .
O4 C8 O3 127.6(2) . .
O4 C8 C3 118.1(2) . .
O3 C8 C3 114.3(2) . .
N2 C9 C10 120.3(3) . .
N2 C9 H9A 119.8 . .
C10 C9 H9A 119.8 . .
C9 C10 C11 119.8(3) . .
C9 C10 H10A 120.1 . .
C11 C10 H10A 120.1 . .
C10 C11 C12 118.8(3) . .
C10 C11 C16 120.8(3) . .
C12 C11 C16 120.4(3) . .
C13 C12 C11 119.1(3) . .
C13 C12 H12A 120.4 . .
C11 C12 H12A 120.4 . .
N2 C13 C12 121.0(3) . .
N2 C13 H13A 119.5 . .
C12 C13 H13A 119.5 . .
N2 C14 C15 110.8(2) . .
N2 C14 H14A 109.5 . .
C15 C14 H14A 109.5 . .
N2 C14 H14B 109.5 . .
C15 C14 H14B 109.5 . .
H14A C14 H14B 108.1 . .
O6 C15 O5 126.6(3) . .
O6 C15 C14 120.7(3) . .
O5 C15 C14 112.7(3) . .
O8 C16 O7 127.5(3) . .
O8 C16 C11 118.5(3) . .
O7 C16 C11 114.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.934(2) 3_657
Cu1 O9 1.957(2) .
Cu1 O9 2.021(2) 3_656
Cu1 Cl1 2.2640(14) .
Cu1 O1 2.359(2) .
Cu1 Cu1 3.0229(14) 3_656
Cu2 O2 1.951(2) .
Cu2 O7 1.957(2) .
Cu2 O5 1.971(2) 4_566
Cu2 O9 1.975(2) .
Cu2 O4 2.287(2) 1_554
O1 C7 1.228(3) .
O2 C7 1.268(3) .
O3 C8 1.255(3) .
O3 Cu1 1.934(2) 3_657
O4 C8 1.230(4) .
O4 Cu2 2.287(2) 1_556
O5 C15 1.268(3) .
O5 Cu2 1.971(2) 4_665
O6 C15 1.223(4) .
O7 C16 1.267(4) .
O8 C16 1.231(4) .
O9 Cu1 2.021(2) 3_656
O9 H99A 0.9800 .
N1 C5 1.336(4) .
N1 C1 1.337(4) .
N1 C6 1.486(3) .
N2 C13 1.337(4) .
N2 C9 1.341(4) .
N2 C14 1.475(4) .
C1 C2 1.379(4) .
C1 H1A 0.9300 .
C2 C3 1.384(4) .
C2 H2A 0.9300 .
C3 C4 1.384(4) .
C3 C8 1.526(3) .
C4 C5 1.378(4) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C6 C7 1.523(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C9 C10 1.376(5) .
C9 H9A 0.9300 .
C10 C11 1.383(4) .
C10 H10A 0.9300 .
C11 C12 1.387(4) .
C11 C16 1.523(4) .
C12 C13 1.376(4) .
C12 H12A 0.9300 .
C13 H13A 0.9300 .
C14 C15 1.532(4) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
