#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/97/7109718.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_7109718
loop_
_publ_author_name
'Sameh K. Elsaidi'
'Mona H. Mohamed'
'Lukasz Wojtas'
'Amy J. Cairns'
'Mohamed Eddaoudi'
'Michael J. Zaworotko'
_publ_section_title
;
 Two-step crystal engineering of porous nets from [Cr/3(mu/3-O)(RCO/2)6]
 and [Cu/3(mu/3-Cl)(RNH2)/6Cl/6] molecular building blocks
;
_journal_name_full               Chem.Commun.
_journal_page_first              8154
_journal_paper_doi               10.1039/c3cc44133d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C126 H161 Cl14 Cr9 Cu6 N18 O65.5'
_chemical_formula_weight         4321.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           193
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2'
_symmetry_space_group_name_H-M   'P 63/m c m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   29.72(2)
_cell_length_b                   29.72(2)
_cell_length_c                   26.388(18)
_cell_measurement_temperature    100(2)
_cell_volume                     20185(2)
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_publication_material  'APEX2 (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40663
_diffrn_reflns_av_R_equivalents  0.1506
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7178
_diffrn_reflns_theta_full        8.06
_diffrn_reflns_theta_max         8.06
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_correction_T_min  0.9873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4390
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Mixture of MeOH and CH2Cl2 solvents have been used. 
Water can be present as well.Possible formula would therefore be 
[(Cr3O)3(H2O)3 (C7H6NO2)18(Cu3ClCl6)2].23.5H2O.(xCH2Cl2,yMeOH,zH2O)
with total number of electrons from x,y,z solcents not exceeding 
1332 per formula unit. 
;
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         1228
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2452
_reflns_number_gt                731
_reflns_number_total             1228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc44133d.txt
_cod_data_source_block           tp-PMBB-6-stp-1_0m
_cod_original_cell_volume        20192(24)
_cod_original_sg_symbol_H-M      P63/mcm
_cod_original_formula_sum        'C126 H161 Cl14 Cr9 Cu6 N18 O65.50'
_cod_database_code               7109718
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z'
'x, x-y, -z'
'-x+y, y, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'y, x, z'
'-x, -x+y, z'
'x-y, -y, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.23654(16) 0.61827(8) 0.5000 0.119(2) Uani 1 2 d S
Cr2 Cr 0.0000 0.5837(3) 0.2500 0.106(3) Uani 1 4 d SDU
Cr3 Cr 0.0000 0.6781(2) 0.3120(2) 0.119(3) Uani 1 2 d SD
Cl1 Cl 0.2136(2) 0.6689(2) 0.5462(2) 0.128(3) Uani 1 1 d .
Cl2 Cl 0.3333 0.6667 0.5000 0.105(5) Uani 1 6 d S
C1 C 0.069(2) 0.7607(18) 0.2500 0.136(11) Uani 1 2 d SDU
C2 C 0.1224(13) 0.8073(12) 0.2500 0.186(13) Uani 1 2 d SDU
O1 O 0.0000 0.5097(10) 0.2500 0.153(13) Uani 1 4 d S
O2 O 0.0521(7) 0.6038(6) 0.2971(7) 0.160(7) Uani 1 1 d DU
O3 O 0.0000 0.7124(7) 0.3836(8) 0.171(10) Uani 1 2 d S
O4 O 0.0000 0.6459(5) 0.2500 0.115(11) Uani 1 4 d SDU
O5 O 0.0538(6) 0.6681(6) 0.3416(6) 0.119(6) Uani 1 1 d DU
O6 O 0.3333 0.6667 0.3598(7) 0.096(8) Uani 1 3 d S
O7 O 0.0522(7) 0.7445(6) 0.2954(7) 0.148(7) Uani 1 1 d DU
N1 N 0.2481(7) 0.6646(7) 0.4370(6) 0.133(7) Uani 1 1 d DU
H1A H 0.2661 0.6988 0.4469 0.159 Uiso 1 1 calc R
H1B H 0.2686 0.6595 0.4143 0.159 Uiso 1 1 calc R
C5 C 0.2004(10) 0.6551(10) 0.4107(9) 0.129(7) Uani 1 1 d DU
C6 C 0.1782(9) 0.6191(8) 0.3729(9) 0.155(9) Uani 1 1 d DU
H6 H 0.1946 0.6001 0.3627 0.185 Uiso 1 1 calc R
C7 C 0.1158(7) 0.6437(6) 0.3587(6) 0.130(8) Uani 1 1 d DU
C8 C 0.1387(8) 0.6798(7) 0.3965(7) 0.133(7) Uani 1 1 d DU
H8 H 0.1244 0.7012 0.4046 0.160 Uiso 1 1 calc R
C9 C 0.1812(9) 0.6866(8) 0.4233(8) 0.139(7) Uani 1 1 d DU
H9 H 0.1964 0.7120 0.4492 0.167 Uiso 1 1 calc R
C10 C 0.1334(9) 0.6095(8) 0.3491(8) 0.148(9) Uani 1 1 d DU
H10 H 0.1152 0.5807 0.3271 0.178 Uiso 1 1 calc R
C11 C 0.0701(6) 0.6383(5) 0.3303(5) 0.123(7) Uani 1 1 d DU
C12 C 0.1976(14) 0.8734(13) 0.2952(4) 0.45(3) Uiso 1 1 d D
H12 H 0.2147 0.8884 0.3263 0.546 Uiso 1 1 calc R
C13 C 0.1482(13) 0.8300(12) 0.2950(4) 0.354 Uiso 1 1 d D
H13 H 0.1316 0.8154 0.3264 0.425 Uiso 1 1 calc R
C14 C 0.2215(19) 0.8944(17) 0.2500 0.46(5) Uiso 1 2 d SD
N15 N 0.275(2) 0.9410(18) 0.2500 0.65(7) Uiso 1 2 d SD
H15A H 0.2904 0.9548 0.2211 0.777 Uiso 0.50 1 calc PR
H15B H 0.2904 0.9548 0.2789 0.777 Uiso 0.50 1 calc PR
O31 O 0.314(2) 1.0000 0.359(3) 0.57(4) Uiso 1 2 d SD
O32 O 0.287(3) 1.0000 0.448(3) 0.53(8) Uiso 0.50 2 d SPD
O33 O 0.232(2) 1.0000 0.376(3) 0.49(5) Uiso 0.75 2 d SPD
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0002 0.0005 '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 0.0004 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0015 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.1580 0.2154 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0535 0.0512 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2418 0.4566 '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
N1 Cu1 N1 163.5(11) 11_566 .
N1 Cu1 Cl1 89.7(6) 11_566 11_566
N1 Cu1 Cl1 94.5(6) . 11_566
N1 Cu1 Cl1 94.5(6) 11_566 .
N1 Cu1 Cl1 89.7(6) . .
Cl1 Cu1 Cl1 150.1(4) 11_566 .
N1 Cu1 Cl2 81.7(5) 11_566 .
N1 Cu1 Cl2 81.7(5) . .
Cl1 Cu1 Cl2 104.96(19) 11_566 .
Cl1 Cu1 Cl2 104.96(19) . .
O2 Cr2 O2 169.0(11) . 8
O2 Cr2 O2 93.7(11) . 23
O2 Cr2 O2 85.3(11) 8 23
O2 Cr2 O2 85.3(11) . 14_556
O2 Cr2 O2 93.7(11) 8 14_556
O2 Cr2 O2 169.0(11) 23 14_556
O2 Cr2 O4 95.5(5) . .
O2 Cr2 O4 95.5(5) 8 .
O2 Cr2 O4 95.5(5) 23 .
O2 Cr2 O4 95.5(5) 14_556 .
O2 Cr2 O1 84.5(5) . .
O2 Cr2 O1 84.5(5) 8 .
O2 Cr2 O1 84.5(5) 23 .
O2 Cr2 O1 84.5(5) 14_556 .
O4 Cr2 O1 180.000(6) . .
O7 Cr3 O7 92.9(10) . 23
O7 Cr3 O4 97.0(6) . .
O7 Cr3 O4 97.0(6) 23 .
O7 Cr3 O5 169.4(7) . 23
O7 Cr3 O5 86.7(7) 23 23
O4 Cr3 O5 93.5(5) . 23
O7 Cr3 O5 86.7(7) . .
O7 Cr3 O5 169.4(7) 23 .
O4 Cr3 O5 93.5(5) . .
O5 Cr3 O5 91.7(10) 23 .
O7 Cr3 O3 84.3(7) . .
O7 Cr3 O3 84.3(7) 23 .
O4 Cr3 O3 178.0(8) . .
O5 Cr3 O3 85.1(6) 23 .
O5 Cr3 O3 85.1(6) . .
Cu1 Cl2 Cu1 120.000(1) 4_565 .
Cu1 Cl2 Cu1 120.000(1) 4_565 3_665
Cu1 Cl2 Cu1 120.000(1) . 3_665
O7 C1 O7 135(5) 14_556 .
O7 C1 C2 113(3) 14_556 .
O7 C1 C2 113(3) . .
C13 C2 C13 117(3) . 14_556
C13 C2 C1 121.4(13) . .
C13 C2 C1 121.4(13) 14_556 .
C11 O2 Cr2 133.6(15) . .
Cr2 O4 Cr3 120.3(4) . .
Cr2 O4 Cr3 120.3(4) . 14_556
Cr3 O4 Cr3 119.3(9) . 14_556
C11 O5 Cr3 131.5(15) . .
C1 O7 Cr3 125(3) . .
C5 N1 Cu1 115.2(14) . .
C5 N1 H1A 108.5 . .
Cu1 N1 H1A 108.5 . .
C5 N1 H1B 108.5 . .
Cu1 N1 H1B 108.5 . .
H1A N1 H1B 107.5 . .
C9 C5 C6 120.8(18) . .
C9 C5 N1 117(2) . .
C6 C5 N1 122(2) . .
C10 C6 C5 122(2) . .
C10 C6 H6 118.8 . .
C5 C6 H6 118.8 . .
C8 C7 C10 119.2(14) . .
C8 C7 C11 121.4(15) . .
C10 C7 C11 119.3(15) . .
C7 C8 C9 123.3(18) . .
C7 C8 H8 118.3 . .
C9 C8 H8 118.3 . .
C5 C9 C8 117(2) . .
C5 C9 H9 121.7 . .
C8 C9 H9 121.7 . .
C6 C10 C7 116.8(19) . .
C6 C10 H10 121.6 . .
C7 C10 H10 121.6 . .
O5 C11 O2 126.4(19) . .
O5 C11 C7 117.6(17) . .
O2 C11 C7 116.0(16) . .
C14 C12 C13 119(2) . .
C14 C12 H12 120.4 . .
C13 C12 H12 120.4 . .
C12 C13 C2 121.5(17) . .
C12 C13 H13 119.2 . .
C2 C13 H13 119.2 . .
C12 C14 C12 121(3) 14_556 .
C12 C14 N15 119.4(17) 14_556 .
C12 C14 N15 119.4(17) . .
C14 N15 H15A 120.0 . .
C14 N15 H15B 120.0 . .
H15A N15 H15B 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.074(15) 11_566
Cu1 N1 2.074(15) .
Cu1 Cl1 2.289(6) 11_566
Cu1 Cl1 2.289(6) .
Cu1 Cl2 2.492(5) .
Cr2 O2 1.837(17) .
Cr2 O2 1.837(17) 8
Cr2 O2 1.837(17) 23
Cr2 O2 1.837(17) 14_556
Cr2 O4 1.848(13) .
Cr2 O1 2.20(3) .
Cr3 O7 1.853(16) .
Cr3 O7 1.853(15) 23
Cr3 O4 1.896(8) .
Cr3 O5 1.932(17) 23
Cr3 O5 1.932(17) .
Cr3 O3 2.15(2) .
Cl2 Cu1 2.492(5) 4_565
Cl2 Cu1 2.492(5) 3_665
C1 O7 1.30(2) 14_556
C1 O7 1.30(2) .
C1 C2 1.49(5) .
C2 C13 1.392(18) .
C2 C13 1.392(18) 14_556
O2 C11 1.247(10) .
O4 Cr3 1.896(8) 14_556
O5 C11 1.242(10) .
N1 C5 1.47(2) .
N1 H1A 0.9200 .
N1 H1B 0.9200 .
C5 C9 1.358(17) .
C5 C6 1.369(17) .
C6 C10 1.367(17) .
C6 H6 0.9500 .
C7 C8 1.370(15) .
C7 C10 1.379(15) .
C7 C11 1.486(16) .
C8 C9 1.371(17) .
C8 H8 0.9500 .
C9 H9 0.9500 .
C10 H10 0.9500 .
C12 C14 1.37(2) .
C12 C13 1.389(19) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 C12 1.37(2) 14_556
C14 N15 1.49(2) .
N15 H15A 0.8800 .
N15 H15B 0.8800 .
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 -0.006 -0.004 -0.008 13353 2633 ' '
