#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/46/7104643.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_7104643
loop_
_publ_author_name
'Mir, Mohammad Hedayetullah'
'Wang, Li'
'Wong, Ming Wah'
'Vittal, Jagadese J'
_publ_section_title
;
 Water helicate (H(2)O)(7), hosted by a diamondoid metal-organic
 framework.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4539
_journal_page_last               4541
_journal_paper_doi               10.1039/b906270j
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C42 H47 Cl2 Cu3 N6 O23.5'
_chemical_formula_weight         1273.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.271(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.791(3)
_cell_length_b                   22.674(3)
_cell_length_c                   12.8770(17)
_cell_measurement_reflns_used    7412
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.24
_cell_volume                     5308.2(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18442
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_T_max  0.6368
_exptl_absorpt_correction_T_min  0.5457
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0746P)²+4.1583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                4517
_reflns_number_total             5213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906270j.txt
_cod_data_source_block           8361jj
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C42 H47 Cl2 Cu3 N6 O23.50'
_cod_database_code               7104643
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.495562(16) 0.761152(13) 0.54798(2) 0.03480(12) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.862118(17) 0.7500 0.03168(13) Uani 1 2 d S . .
O1 O 0.57769(11) 0.74239(8) 0.68852(16) 0.0435(5) Uani 1 1 d . . .
O2 O 0.57671(9) 0.80480(8) 0.82350(15) 0.0371(4) Uani 1 1 d . . .
O3 O 0.51219(10) 0.84678(8) 0.55999(15) 0.0369(4) Uani 1 1 d . . .
O4 O 0.62719(12) 0.84826(9) 0.5672(2) 0.0565(6) Uani 1 1 d . . .
N1 N 0.40429(12) 0.76683(10) 0.40790(19) 0.0400(5) Uani 1 1 d . . .
N2 N 0.46563(13) 0.67583(10) 0.53259(19) 0.0404(5) Uani 1 1 d . . .
N3 N 0.57098(12) 0.92887(9) 0.79993(17) 0.0362(5) Uani 1 1 d . . .
C1 C 0.37500(16) 0.81625(15) 0.3509(3) 0.0517(7) Uani 1 1 d . . .
H1 H 0.3968 0.8527 0.3802 0.062 Uiso 1 1 calc R . .
C2 C 0.31381(19) 0.8152(2) 0.2504(3) 0.0695(10) Uani 1 1 d . . .
H2 H 0.2937 0.8506 0.2129 0.083 Uiso 1 1 calc R . .
C3 C 0.2830(2) 0.7629(2) 0.2063(3) 0.0799(12) Uani 1 1 d . . .
H3 H 0.2419 0.7614 0.1371 0.096 Uiso 1 1 calc R . .
C4 C 0.3125(2) 0.7117(2) 0.2638(3) 0.0706(10) Uani 1 1 d . . .
H4 H 0.2917 0.6750 0.2340 0.085 Uiso 1 1 calc R . .
C5 C 0.37286(15) 0.71451(14) 0.3656(2) 0.0455(6) Uani 1 1 d . . .
C6 C 0.40732(16) 0.66316(13) 0.4363(3) 0.0469(7) Uani 1 1 d . . .
C7 C 0.3835(2) 0.60575(16) 0.4097(3) 0.0658(9) Uani 1 1 d . . .
H7 H 0.3430 0.5974 0.3421 0.079 Uiso 1 1 calc R . .
C8 C 0.4192(2) 0.56084(16) 0.4826(4) 0.0745(11) Uani 1 1 d . . .
H8 H 0.4033 0.5216 0.4657 0.089 Uiso 1 1 calc R . .
C9 C 0.4784(2) 0.57399(14) 0.5803(4) 0.0658(9) Uani 1 1 d . . .
H9 H 0.5036 0.5440 0.6313 0.079 Uiso 1 1 calc R . .
C10 C 0.50056(19) 0.63184(13) 0.6027(3) 0.0516(7) Uani 1 1 d . . .
H10 H 0.5415 0.6408 0.6693 0.062 Uiso 1 1 calc R . .
C11 C 0.64426(15) 0.92379(14) 0.8483(2) 0.0477(7) Uani 1 1 d . . .
H11 H 0.6654 0.8860 0.8652 0.057 Uiso 1 1 calc R . .
C12 C 0.68973(18) 0.97286(17) 0.8741(3) 0.0617(9) Uani 1 1 d . . .
H12 H 0.7411 0.9684 0.9079 0.074 Uiso 1 1 calc R . .
C13 C 0.6591(2) 1.02738(16) 0.8501(3) 0.0625(9) Uani 1 1 d . . .
H13 H 0.6893 1.0610 0.8672 0.075 Uiso 1 1 calc R . .
C14 C 0.5834(2) 1.03325(13) 0.8003(3) 0.0519(8) Uani 1 1 d . . .
H14 H 0.5616 1.0708 0.7829 0.062 Uiso 1 1 calc R . .
C15 C 0.54023(15) 0.98282(11) 0.7764(2) 0.0380(6) Uani 1 1 d . . .
C16 C 0.60351(13) 0.76330(10) 0.7859(2) 0.0331(5) Uani 1 1 d . . .
C17 C 0.67324(14) 0.73675(11) 0.8655(2) 0.0376(6) Uani 1 1 d . . .
H17 H 0.6884 0.7005 0.8464 0.045 Uiso 1 1 calc R . .
C18 C 0.71499(13) 0.76198(11) 0.9622(2) 0.0354(5) Uani 1 1 d . . .
H18A H 0.6984 0.7972 0.9829 0.042 Uiso 1 1 calc R . .
C19 C 0.56920(15) 0.87300(11) 0.5588(2) 0.0382(6) Uani 1 1 d . . .
C20 C 0.56483(15) 0.93821(12) 0.5463(2) 0.0394(6) Uani 1 1 d . . .
H20 H 0.6090 0.9594 0.5668 0.047 Uiso 1 1 calc R . .
C21 C 0.50203(15) 0.96830(11) 0.5078(2) 0.0373(5) Uani 1 1 d . . .
H21 H 0.4579 0.9473 0.4898 0.045 Uiso 1 1 calc R . .
O5 O 0.56874(14) 0.74907(11) 0.4450(2) 0.0588(6) Uani 1 1 d D . .
H5A H 0.590(2) 0.7160(11) 0.462(4) 0.080 Uiso 1 1 d D . .
H5B H 0.6051(18) 0.7697(17) 0.485(3) 0.080 Uiso 1 1 d D . .
O1W O 0.5000 0.82784(16) 0.2500 0.0613(8) Uani 1 2 d SD . .
H1W H 0.5252(18) 0.8055(13) 0.300(2) 0.056(10) Uiso 1 1 d D . .
O2W O 0.75691(16) 0.89614(12) 0.5806(3) 0.0866(9) Uani 1 1 d D . .
H2WA H 0.7112(13) 0.8843(18) 0.558(3) 0.080 Uiso 1 1 d D . .
H2WB H 0.764(2) 0.9333(9) 0.591(4) 0.080 Uiso 1 1 d D . .
O3W O 0.6447(3) 0.6464(2) 0.4962(5) 0.1372(17) Uani 1 1 d D . .
H3WA H 0.644(3) 0.6279(18) 0.556(3) 0.080 Uiso 1 1 d D . .
H3WB H 0.677(2) 0.6340(18) 0.473(4) 0.080 Uiso 1 1 d D . .
Cl1 Cl 0.79604(6) 0.94869(4) 0.19777(9) 0.0718(3) Uani 1 1 d . . .
O6 O 0.8184(2) 0.9333(2) 0.3136(3) 0.1375(17) Uani 1 1 d D A .
O7 O 0.7236(6) 0.9676(7) 0.1534(7) 0.152(6) Uani 0.67(2) 1 d PD A 1
O8 O 0.8405(7) 0.9961(4) 0.1859(9) 0.165(4) Uani 0.67(2) 1 d PD A 1
O9 O 0.8055(8) 0.9027(3) 0.1360(10) 0.158(5) Uani 0.67(2) 1 d PD A 1
O7A O 0.7242(11) 0.9295(13) 0.1443(12) 0.152(12) Uani 0.33(2) 1 d PD A 2
O8A O 0.7926(18) 1.0096(5) 0.2040(13) 0.150(11) Uani 0.33(2) 1 d PD A 2
O9A O 0.8383(14) 0.9304(16) 0.1551(19) 0.202(16) Uani 0.33(2) 1 d PD A 2
O1S O 0.5000 0.4133(10) 0.7500 0.105(6) Uiso 0.25 2 d SP . .
O2S O 0.5000 0.3574(10) 0.7500 0.107(6) Uiso 0.25 2 d SP . .
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
_geom_angle_publ_flag
O1 Cu1 O3 95.20(8) . . ?
O1 Cu1 N1 169.91(9) . . ?
O3 Cu1 N1 94.09(9) . . ?
O1 Cu1 N2 89.23(9) . . ?
O3 Cu1 N2 172.93(8) . . ?
N1 Cu1 N2 81.15(10) . . ?
O1 Cu1 O5 91.44(9) . . ?
O3 Cu1 O5 92.20(8) . . ?
N1 Cu1 O5 92.13(9) . . ?
N2 Cu1 O5 93.20(9) . . ?
O2 Cu2 O2 95.75(11) 2_656 . ?
O2 Cu2 N3 169.86(8) 2_656 . ?
O2 Cu2 N3 92.03(8) . . ?
O2 Cu2 N3 92.03(8) 2_656 2_656 ?
O2 Cu2 N3 169.86(8) . 2_656 ?
N3 Cu2 N3 81.04(13) . 2_656 ?
C16 O1 Cu1 135.55(17) . . ?
C16 O2 Cu2 132.63(17) . . ?
C19 O3 Cu1 125.35(16) . . ?
C1 N1 C5 118.9(3) . . ?
C1 N1 Cu1 126.3(2) . . ?
C5 N1 Cu1 114.67(19) . . ?
C10 N2 C6 119.1(3) . . ?
C10 N2 Cu1 126.6(2) . . ?
C6 N2 Cu1 114.0(2) . . ?
C11 N3 C15 119.6(2) . . ?
C11 N3 Cu2 125.57(19) . . ?
C15 N3 Cu2 114.80(17) . . ?
N1 C1 C2 121.9(3) . . ?
C3 C2 C1 119.5(4) . . ?
C2 C3 C4 119.3(3) . . ?
C3 C4 C5 119.7(4) . . ?
N1 C5 C4 120.7(3) . . ?
N1 C5 C6 114.8(2) . . ?
C4 C5 C6 124.5(3) . . ?
N2 C6 C7 120.9(3) . . ?
N2 C6 C5 114.8(2) . . ?
C7 C6 C5 124.3(3) . . ?
C8 C7 C6 119.6(3) . . ?
C9 C8 C7 119.2(3) . . ?
C8 C9 C10 119.0(4) . . ?
N2 C10 C9 122.1(3) . . ?
N3 C11 C12 121.6(3) . . ?
C13 C12 C11 119.2(3) . . ?
C12 C13 C14 119.8(3) . . ?
C13 C14 C15 118.9(3) . . ?
N3 C15 C14 121.0(3) . . ?
N3 C15 C15 114.62(14) . 2_656 ?
C14 C15 C15 124.37(19) . 2_656 ?
O1 C16 O2 126.9(2) . . ?
O1 C16 C17 116.2(2) . . ?
O2 C16 C17 116.9(2) . . ?
C18 C17 C16 122.7(2) . . ?
C17 C18 C18 123.1(3) . 7_667 ?
O4 C19 O3 125.2(2) . . ?
O4 C19 C20 118.1(2) . . ?
O3 C19 C20 116.7(2) . . ?
C21 C20 C19 123.8(3) . . ?
C20 C21 C21 123.6(3) . 5_676 ?
O9A Cl1 O9 38.5(17) . . ?
O9A Cl1 O7A 114.5(11) . . ?
O9 Cl1 O7A 79.6(13) . . ?
O9A Cl1 O7 133.7(12) . . ?
O9 Cl1 O7 110.6(6) . . ?
O7A Cl1 O7 36.8(10) . . ?
O9A Cl1 O8A 114.5(10) . . ?
O9 Cl1 O8A 144.4(11) . . ?
O7A Cl1 O8A 106.2(9) . . ?
O7 Cl1 O8A 69.5(10) . . ?
O9A Cl1 O6 113.4(9) . . ?
O9 Cl1 O6 111.5(5) . . ?
O7A Cl1 O6 106.2(6) . . ?
O7 Cl1 O6 110.6(4) . . ?
O8A Cl1 O6 100.7(8) . . ?
O9A Cl1 O8 69.7(15) . . ?
O9 Cl1 O8 106.2(5) . . ?
O7A Cl1 O8 137.4(8) . . ?
O7 Cl1 O8 107.7(5) . . ?
O8A Cl1 O8 46.1(12) . . ?
O6 Cl1 O8 110.2(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.9426(19) . ?
Cu1 O3 1.9650(18) . ?
Cu1 N1 1.990(2) . ?
Cu1 N2 2.010(2) . ?
Cu1 O5 2.335(2) . ?
Cu2 O2 1.9376(17) 2_656 ?
Cu2 O2 1.9376(17) . ?
Cu2 N3 1.991(2) . ?
Cu2 N3 1.991(2) 2_656 ?
O1 C16 1.246(3) . ?
O2 C16 1.266(3) . ?
O3 C19 1.281(3) . ?
O4 C19 1.243(3) . ?
N1 C1 1.340(4) . ?
N1 C5 1.350(4) . ?
N2 C10 1.339(4) . ?
N2 C6 1.349(4) . ?
N3 C11 1.338(4) . ?
N3 C15 1.346(3) . ?
C1 C2 1.380(5) . ?
C2 C3 1.352(6) . ?
C3 C4 1.375(6) . ?
C4 C5 1.383(4) . ?
C5 C6 1.469(4) . ?
C6 C7 1.381(4) . ?
C7 C8 1.377(6) . ?
C8 C9 1.371(6) . ?
C9 C10 1.377(4) . ?
C11 C12 1.386(4) . ?
C12 C13 1.357(5) . ?
C13 C14 1.384(5) . ?
C14 C15 1.387(4) . ?
C15 C15 1.464(6) 2_656 ?
C16 C17 1.483(3) . ?
C17 C18 1.322(4) . ?
C18 C18 1.448(5) 7_667 ?
C19 C20 1.486(4) . ?
C20 C21 1.330(4) . ?
C21 C21 1.449(5) 5_676 ?
Cl1 O9A 1.240(14) . ?
Cl1 O9 1.369(8) . ?
Cl1 O7A 1.382(14) . ?
Cl1 O7 1.385(8) . ?
Cl1 O8A 1.387(12) . ?
Cl1 O6 1.421(4) . ?
Cl1 O8 1.435(7) . ?
O1S O2S 1.27(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O4 0.844(19) 2.03(3) 2.727(3) 140(4) .
O5 H5A O3W 0.843(19) 1.87(2) 2.707(4) 173(4) .
O1W H1W O5 0.814(18) 2.15(2) 2.940(3) 165(4) .
O2W H2WA O4 0.876(19) 1.90(2) 2.729(3) 157(4) .
O2W H2WB O8A 0.858(19) 1.86(3) 2.589(14) 142(4) 6_576
O2W H2WB O8 0.858(19) 2.21(3) 2.963(14) 147(4) 6_576
O2W H2WB O7 0.858(19) 2.62(3) 3.369(16) 147(4) 6_576
O3W H3WA O6 0.880(19) 2.08(3) 2.897(6) 154(4) 7_666
O3W H3WB O2W 0.853(19) 1.83(2) 2.687(5) 177(4) 7_666
