#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/13/4001385.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_4001385
loop_
_publ_author_name
'Wang, Xin-Yi'
'Scancella, Michael'
'Sevov, Slavi C.'
_publ_section_title
;
 Studies of the Mechanism of a Single-Crystal-to-Single-Crystal Reversible
 Dehydration of a Copper Carboxylate Framework
;
_journal_issue                   18
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4506
_journal_paper_doi               10.1021/cm071005z
_journal_volume                  19
_journal_year                    2007
_chemical_formula_moiety         'C16 H20 Cl2 Cu7 O26, 2(H2 O)'
_chemical_formula_sum            'C16 H24 Cl2 Cu7 O28'
_chemical_formula_weight         1180.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.8030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2604(2)
_cell_length_b                   10.1663(2)
_cell_length_c                   10.5637(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1530.72(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    Diomand
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16935
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    5.060
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R.H. (1995) Acta Cryst. A51, 33-38'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0252
_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)+(0.0290P)²+1.3119P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                2959
_reflns_number_total             3510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071005zsi20070614_034201.cif
_cod_data_source_block           1-CuTHFTCasmade
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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      P2(1)/c
_cod_database_code               4001385
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.5000 1.0000 0.5000 0.01106(11) Uani 1 2 d S
Cu5 Cu 0.5000 0.5000 0.5000 0.01010(11) Uani 1 2 d S
O1 O 0.34366(12) 0.97825(17) 0.53733(18) 0.0082(4) Uani 1 1 d .
O2 O 0.49916(13) 0.98464(19) 0.6868(2) 0.0151(4) Uani 1 1 d .
O3 O 0.41871(12) 1.04445(19) 0.85600(19) 0.0138(4) Uani 1 1 d .
O4 O 0.12464(12) 1.07462(18) 0.76046(18) 0.0111(4) Uani 1 1 d .
O5 O 0.12910(12) 0.97364(17) 0.57099(18) 0.0092(4) Uani 1 1 d .
O6 O 0.13081(12) 0.72740(17) 0.73036(18) 0.0094(4) Uani 1 1 d .
O7 O 0.19016(12) 0.63898(18) 0.55445(19) 0.0112(4) Uani 1 1 d .
O8 O 0.40557(12) 0.63671(18) 0.5359(2) 0.0148(4) Uani 1 1 d .
O9 O 0.48698(12) 0.81212(19) 0.4806(2) 0.0163(5) Uani 1 1 d .
C1 C 0.33297(17) 1.0275(2) 0.6641(3) 0.0081(5) Uani 1 1 d .
H1 H 0.314(2) 1.124(3) 0.651(3) 0.022(3) Uiso 1 1 d .
C2 C 0.25598(16) 0.9422(3) 0.7203(3) 0.0071(5) Uani 1 1 d .
H2 H 0.261(2) 0.935(3) 0.807(3) 0.022(3) Uiso 1 1 d .
C3 C 0.27628(17) 0.8077(2) 0.6615(3) 0.0080(5) Uani 1 1 d .
H3 H 0.318(2) 0.763(3) 0.711(3) 0.022(3) Uiso 1 1 d .
C4 C 0.32423(17) 0.8382(2) 0.5369(3) 0.0084(5) Uani 1 1 d .
H4 H 0.281(2) 0.825(3) 0.461(3) 0.022(3) Uiso 1 1 d .
C5 C 0.42552(18) 1.0178(2) 0.7410(3) 0.0094(5) Uani 1 1 d .
C6 C 0.16057(17) 1.0004(2) 0.6799(3) 0.0080(5) Uani 1 1 d .
C7 C 0.19122(16) 0.7175(2) 0.6469(3) 0.0080(5) Uani 1 1 d .
C8 C 0.41338(17) 0.7563(3) 0.5175(3) 0.0100(5) Uani 1 1 d .
Cu3 Cu 0.00098(2) 0.65424(3) 0.73643(3) 0.00692(9) Uani 1 1 d .
Cu4 Cu 0.10132(2) 0.49776(3) 0.52568(3) 0.00779(9) Uani 1 1 d .
O11 O 0.00609(12) 0.38367(18) 0.44746(19) 0.0074(4) Uani 1 1 d .
O1W O 0.20379(13) 0.3706(2) 0.5056(2) 0.0146(4) Uani 1 1 d D
Cl1 Cl 0.07375(4) 0.39960(6) 0.76456(7) 0.01154(14) Uani 1 1 d .
H1W1 H 0.204(2) 0.337(3) 0.4267(19) 0.022(3) Uiso 1 1 d D
H1W2 H 0.2612(15) 0.386(3) 0.540(3) 0.022(3) Uiso 1 1 d D
H111 H 0.004(2) 0.331(4) 0.481(4) 0.022(3) Uiso 1 1 d .
O10 O 0.01864(12) 0.66662(18) 0.91882(19) 0.0080(4) Uani 1 1 d .
H101 H 0.065(2) 0.681(3) 0.920(4) 0.022(3) Uiso 1 1 d .
Cu2 Cu 0.0000 0.5000 1.0000 0.00705(10) Uani 1 2 d S
O3W O 0.28269(17) 0.1641(3) 0.3341(3) 0.0394(7) Uani 1 1 d D
H3W1 H 0.3081(19) 0.139(3) 0.242(2) 0.022(3) Uiso 1 1 d D
H3W2 H 0.2201(13) 0.134(3) 0.311(3) 0.022(3) Uiso 1 1 d D
O2W O 0.38408(15) 0.3645(2) 0.6036(2) 0.0228(5) Uani 1 1 d D
H2W1 H 0.379(3) 0.375(3) 0.6956(19) 0.036(11) Uiso 1 1 d D
H2W2 H 0.423(3) 0.285(3) 0.599(4) 0.086(18) Uiso 1 1 d 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'
Cu Cu 0.3201 1.2651 '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'
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
O9 Cu1 O9 179.999(15) 3_676 .
O9 Cu1 O2 88.62(9) 3_676 .
O9 Cu1 O2 91.38(9) . .
O9 Cu1 O2 91.38(9) 3_676 3_676
O9 Cu1 O2 88.62(9) . 3_676
O2 Cu1 O2 180.0 . 3_676
O9 Cu1 O1 80.30(7) 3_676 3_676
O9 Cu1 O1 99.70(7) . 3_676
O2 Cu1 O1 102.47(7) . 3_676
O2 Cu1 O1 77.53(7) 3_676 3_676
O9 Cu1 O1 99.70(7) 3_676 .
O9 Cu1 O1 80.30(7) . .
O2 Cu1 O1 77.53(7) . .
O2 Cu1 O1 102.47(7) 3_676 .
O1 Cu1 O1 180.0 3_676 .
O3 Cu5 O3 180.00(11) 2_646 4_575
O3 Cu5 O8 94.57(8) 2_646 .
O3 Cu5 O8 85.43(8) 4_575 .
O3 Cu5 O8 85.43(8) 2_646 3_666
O3 Cu5 O8 94.57(8) 4_575 3_666
O8 Cu5 O8 180.0 . 3_666
O3 Cu5 O2W 100.19(8) 2_646 .
O3 Cu5 O2W 79.81(8) 4_575 .
O8 Cu5 O2W 80.54(8) . .
O8 Cu5 O2W 99.46(8) 3_666 .
O3 Cu5 O2W 79.81(8) 2_646 3_666
O3 Cu5 O2W 100.19(8) 4_575 3_666
O8 Cu5 O2W 99.46(8) . 3_666
O8 Cu5 O2W 80.54(8) 3_666 3_666
O2W Cu5 O2W 180.0 . 3_666
C1 O1 C4 108.5(2) . .
C1 O1 Cu1 104.99(13) . .
C4 O1 Cu1 106.35(13) . .
C5 O2 Cu1 117.64(18) . .
C5 O3 Cu5 130.47(17) . 2_656
C6 O4 Cu3 130.44(17) . 2_556
C6 O5 Cu2 128.29(16) . 2_556
C7 O6 Cu3 130.49(17) . .
C7 O7 Cu4 125.73(17) . .
C8 O8 Cu5 126.49(17) . .
C8 O9 Cu1 119.27(16) . .
O1 C1 C5 110.8(2) . .
O1 C1 C2 105.2(2) . .
C5 C1 C2 112.0(2) . .
C6 C2 C1 108.3(2) . .
C6 C2 C3 114.1(2) . .
C1 C2 C3 101.6(2) . .
C7 C3 C4 114.2(2) . .
C7 C3 C2 114.7(2) . .
C4 C3 C2 105.2(2) . .
O1 C4 C3 106.6(2) . .
O1 C4 C8 111.91(19) . .
C3 C4 C8 113.4(2) . .
O3 C5 O2 126.3(3) . .
O3 C5 C1 114.2(2) . .
O2 C5 C1 119.6(2) . .
O5 C6 O4 127.6(2) . .
O5 C6 C2 117.5(2) . .
O4 C6 C2 114.8(2) . .
O6 C7 O7 127.0(2) . .
O6 C7 C3 116.2(2) . .
O7 C7 C3 116.7(2) . .
O8 C8 O9 124.7(2) . .
O8 C8 C4 115.6(2) . .
O9 C8 C4 119.7(2) . .
O10 Cu3 O4 95.74(8) . 2_546
O10 Cu3 O11 171.27(8) . 3_566
O4 Cu3 O11 85.30(8) 2_546 3_566
O10 Cu3 O6 85.19(8) . .
O4 Cu3 O6 177.41(8) 2_546 .
O11 Cu3 O6 93.42(8) 3_566 .
O10 Cu3 Cl1 89.02(6) . 2_556
O4 Cu3 Cl1 91.18(6) 2_546 2_556
O11 Cu3 Cl1 99.63(6) 3_566 2_556
O6 Cu3 Cl1 91.25(5) . 2_556
O7 Cu4 O11 162.37(9) . .
O7 Cu4 O1W 91.13(8) . .
O11 Cu4 O1W 94.19(8) . .
O7 Cu4 O11 91.81(8) . 3_566
O11 Cu4 O11 83.75(8) . 3_566
O1W Cu4 O11 176.10(8) . 3_566
O7 Cu4 Cl1 103.71(6) . .
O11 Cu4 Cl1 93.16(6) . .
O1W Cu4 Cl1 89.34(6) . .
O11 Cu4 Cl1 87.47(6) 3_566 .
O7 Cu4 Cu4 131.06(6) . 3_566
O11 Cu4 Cu4 42.22(5) . 3_566
O1W Cu4 Cu4 136.32(6) . 3_566
O11 Cu4 Cu4 41.52(5) 3_566 3_566
Cl1 Cu4 Cu4 90.396(19) . 3_566
Cu4 O11 Cu4 96.25(8) . 3_566
Cu4 O11 Cu3 123.02(10) . 3_566
Cu4 O11 Cu3 104.11(9) 3_566 3_566
Cu3 Cl1 Cu4 113.40(2) 2_546 .
Cu2 O10 Cu3 111.77(9) . .
O10 Cu2 O10 180.0 3_567 .
O10 Cu2 O5 84.83(8) 3_567 2_546
O10 Cu2 O5 95.17(8) . 2_546
O10 Cu2 O5 95.17(8) 3_567 4_576
O10 Cu2 O5 84.82(8) . 4_576
O5 Cu2 O5 180.0 2_546 4_576
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O9 1.9293(19) 3_676
Cu1 O9 1.9293(19) .
Cu1 O2 1.980(2) .
Cu1 O2 1.980(2) 3_676
Cu1 O1 2.2870(17) 3_676
Cu1 O1 2.2870(17) .
Cu5 O3 1.9367(19) 2_646
Cu5 O3 1.9368(19) 4_575
Cu5 O8 1.9802(18) .
Cu5 O8 1.9802(18) 3_666
Cu5 O2W 2.437(2) .
Cu5 O2W 2.437(2) 3_666
O1 C1 1.442(3) .
O1 C4 1.450(3) .
O2 C5 1.258(3) .
O3 C5 1.252(3) .
O3 Cu5 1.9368(19) 2_656
O4 C6 1.258(3) .
O4 Cu3 1.9671(17) 2_556
O5 C6 1.252(3) .
O5 Cu2 1.9840(17) 2_556
O6 C7 1.256(3) .
O6 Cu3 1.9982(17) .
O7 C7 1.261(3) .
O7 Cu4 1.9324(18) .
O8 C8 1.237(3) .
O9 C8 1.265(3) .
C1 C5 1.531(4) .
C1 C2 1.533(3) .
C2 C6 1.532(3) .
C2 C3 1.534(4) .
C3 C7 1.524(3) .
C3 C4 1.534(4) .
C4 C8 1.539(3) .
Cu3 O10 1.939(2) .
Cu3 O4 1.9671(17) 2_546
Cu3 O11 1.980(2) 3_566
Cu3 Cl1 2.7125(7) 2_556
Cu4 O11 1.9498(19) .
Cu4 O1W 1.9676(19) .
Cu4 O11 1.9766(18) 3_566
Cu4 Cl1 2.7534(8) .
Cu4 Cu4 2.9237(6) 3_566
O11 Cu4 1.9766(18) 3_566
O11 Cu3 1.980(2) 3_566
Cl1 Cu3 2.7124(7) 2_546
O10 Cu2 1.9209(18) .
Cu2 O10 1.9209(18) 3_567
Cu2 O5 1.9840(17) 2_546
Cu2 O5 1.9840(17) 4_576
