#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/16/7221690.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_7221690
loop_
_publ_author_name
'Lee, Jae Hwa'
'Kim, Tae Kyung'
'Suh, Myunghyun Paik'
'Moon, Hoi Ri'
_publ_section_title
;
 Solvent-induced single-crystal to single-crystal transformation of a
 Zn4O-containing doubly interpenetrated metal--organic framework with a
 pcu net
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8807
_journal_paper_doi               10.1039/C5CE01074H
_journal_volume                  17
_journal_year                    2015
_chemical_compound_source
'Zinc nitrate hexahydrate, bis(4-carboxyphenyl)-N-methylamine'
_chemical_formula_moiety         'C45 H33 N3 O13 Zn4, 3(C3 H7), 3(C3 H7)'
_chemical_formula_sum            'C63 H75 N3 O13 Zn4'
_chemical_formula_weight         1343.74
_chemical_name_common            Zn4OCPMA_hexane
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-25 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   18.653(3)
_cell_length_b                   18.653(3)
_cell_length_c                   65.066(13)
_cell_measurement_reflns_used    157199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.803
_cell_measurement_theta_min      2.274
_cell_volume                     19606(6)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'MS modeling'
_computing_publication_material  WinGX
_computing_structure_refinement  'Bruker SHELXTL-XL'
_computing_structure_solution    'Bruker SHELXTL-XS'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67999
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       94
_diffrn_reflns_limit_l_min       -94
_diffrn_reflns_number            77769
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.7220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Length, width, and breadth roughly equal'
_exptl_crystal_F_000             8376
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.345
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00350(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         8067
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0575
_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)+(0.1335P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                5700
_reflns_number_total             8067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01074h2.cif
_cod_data_source_block           zn4ocpma_hx_r-3c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7221688--7221691.cif.
;
_cod_original_cell_volume        19605(6)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7221690
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Zn1 Zn 0.3333 0.6667 0.221467(6) 0.03421(13) Uani 1 3 d S
Zn2 Zn 0.359613(14) 0.584346(13) 0.260999(3) 0.03355(11) Uani 1 1 d .
N1 N 0.44921(12) 0.34215(13) 0.16590(3) 0.0468(5) Uani 1 1 d .
O1 O 0.3333 0.6667 0.25120(4) 0.0329(5) Uani 1 3 d S
O2 O 0.38177(11) 0.60353(11) 0.21113(3) 0.0440(4) Uani 1 1 d .
O3 O 0.39276(10) 0.53742(10) 0.23881(2) 0.0416(3) Uani 1 1 d .
O4 O 0.11436(10) 0.14577(10) 0.11469(2) 0.0407(3) Uani 1 1 d .
O5 O 0.17474(9) 0.07053(9) 0.10678(2) 0.0387(3) Uani 1 1 d .
C1 C 0.39688(13) 0.55177(13) 0.21969(3) 0.0397(4) Uani 1 1 d .
C2 C 0.41899(13) 0.50201(13) 0.20592(3) 0.0391(4) Uani 1 1 d .
C3 C 0.42992(14) 0.43887(14) 0.21389(3) 0.0412(4) Uani 1 1 d .
H3 H 0.4294 0.4312 0.2283 0.037(6) Uiso 1 1 calc R
C4 C 0.44161(13) 0.38704(14) 0.20068(3) 0.0410(4) Uani 1 1 d .
H4 H 0.4482 0.3434 0.2061 0.055(8) Uiso 1 1 calc R
C5 C 0.44362(13) 0.39874(14) 0.17961(3) 0.0418(5) Uani 1 1 d .
C6 C 0.43818(16) 0.46555(15) 0.17165(4) 0.0444(5) Uani 1 1 d .
H6 H 0.4432 0.4758 0.1573 0.059(8) Uiso 1 1 calc R
C7 C 0.42543(14) 0.51671(14) 0.18477(4) 0.0433(5) Uani 1 1 d .
H7 H 0.4211 0.5617 0.1794 0.040(6) Uiso 1 1 calc R
C8 C 0.51629(16) 0.32450(18) 0.16905(4) 0.0523(6) Uani 1 1 d .
H8A H 0.4936 0.2681 0.1743 0.046(7) Uiso 1 1 calc R
H8B H 0.5559 0.3640 0.1790 0.069(9) Uiso 1 1 calc R
H8C H 0.5444 0.3296 0.1559 0.090(12) Uiso 1 1 calc R
C9 C 0.17376(13) 0.13101(13) 0.11566(3) 0.0364(4) Uani 1 1 d .
C10 C 0.24618(13) 0.18732(13) 0.12830(3) 0.0373(4) Uani 1 1 d .
C11 C 0.24432(14) 0.24733(14) 0.14058(3) 0.0423(5) Uani 1 1 d .
H11 H 0.1968 0.2536 0.1404 0.048(7) Uiso 1 1 calc R
C12 C 0.31016(14) 0.29789(15) 0.15304(4) 0.0443(5) Uani 1 1 d .
H12 H 0.3067 0.3374 0.1616 0.057(8) Uiso 1 1 calc R
C13 C 0.38252(14) 0.29195(14) 0.15337(3) 0.0404(4) Uani 1 1 d .
C14 C 0.38463(14) 0.23218(15) 0.14069(4) 0.0432(5) Uani 1 1 d .
H14 H 0.4327 0.2269 0.1405 0.074(10) Uiso 1 1 calc R
C15 C 0.31781(13) 0.18093(13) 0.12851(4) 0.0409(4) Uani 1 1 d .
H15 H 0.3205 0.1406 0.1201 0.040(6) Uiso 1 1 calc R
C16 C 0.4851(11) 0.0972(10) 0.1314(2) 0.137(6) Uani 0.50 1 d PD
H16A H 0.4489 0.1189 0.1353 0.206 Uiso 0.50 1 calc PR
H16B H 0.5254 0.1084 0.1423 0.206 Uiso 0.50 1 calc PR
H16C H 0.4518 0.0374 0.1291 0.206 Uiso 0.50 1 calc PR
C17 C 0.5325(19) 0.141(3) 0.1109(3) 0.49(4) Uani 0.50 1 d PDU
H17A H 0.5680 0.2009 0.1134 0.582 Uiso 0.50 1 calc PR
H17B H 0.5686 0.1183 0.1068 0.582 Uiso 0.50 1 calc PR
C18 C 0.4710(13) 0.1264(14) 0.0935(2) 0.206(11) Uani 0.50 1 d PD
H18A H 0.4201 0.1210 0.0997 0.247 Uiso 0.50 1 calc PR
H18B H 0.4557 0.0729 0.0869 0.247 Uiso 0.50 1 calc PR
C19 C 0.501(3) 0.194(2) 0.0763(4) 0.50(4) Uani 0.50 1 d PDU
H19A H 0.4878 0.2376 0.0803 0.598 Uiso 0.50 1 calc PR
H19B H 0.5612 0.2200 0.0744 0.598 Uiso 0.50 1 calc PR
C20 C 0.4544(13) 0.1507(12) 0.05609(18) 0.177(9) Uani 0.50 1 d PD
H20A H 0.4566 0.0998 0.0531 0.213 Uiso 0.50 1 calc PR
H20B H 0.3963 0.1386 0.0560 0.213 Uiso 0.50 1 calc PR
C21 C 0.509(2) 0.2211(17) 0.0421(6) 0.32(2) Uani 0.50 1 d PDU
H21A H 0.4960 0.2655 0.0435 0.473 Uiso 0.50 1 calc PR
H21B H 0.5002 0.2015 0.0278 0.473 Uiso 0.50 1 calc PR
H21C H 0.5673 0.2421 0.0458 0.473 Uiso 0.50 1 calc PR
C22 C 0.2636(8) 0.1606(8) 0.05458(19) 0.139(8) Uani 0.50 1 d PD
H22A H 0.3184 0.1795 0.0486 0.208 Uiso 0.50 1 calc PR
H22B H 0.2217 0.1388 0.0437 0.208 Uiso 0.50 1 calc PR
H22C H 0.2514 0.1169 0.0647 0.208 Uiso 0.50 1 calc PR
C23 C 0.2627(6) 0.2307(10) 0.06484(19) 0.171(12) Uani 0.50 1 d PD
H23A H 0.2167 0.2080 0.0749 0.205 Uiso 0.50 1 calc PR
H23B H 0.2502 0.2614 0.0544 0.205 Uiso 0.50 1 calc PR
C24 C 0.3403(6) 0.2912(7) 0.07585(18) 0.099(4) Uani 0.50 1 d PD
H24A H 0.3855 0.3178 0.0656 0.118 Uiso 0.50 1 calc PR
H24B H 0.3556 0.2601 0.0855 0.118 Uiso 0.50 1 calc PR
C25 C 0.3352(8) 0.3602(7) 0.08800(17) 0.103(5) Uani 0.50 1 d PD
H25A H 0.3164 0.3886 0.0784 0.124 Uiso 0.50 1 calc PR
H25B H 0.2919 0.3332 0.0986 0.124 Uiso 0.50 1 calc PR
C26 C 0.4118(7) 0.4243(7) 0.0982(2) 0.099(4) Uani 0.50 1 d PD
H26A H 0.4561 0.4498 0.0878 0.119 Uiso 0.50 1 calc PR
H26B H 0.4292 0.3966 0.1084 0.119 Uiso 0.50 1 calc PR
C27 C 0.4056(16) 0.4936(18) 0.1092(4) 0.34(2) Uani 0.50 1 d PDU
H27A H 0.3657 0.5042 0.1020 0.506 Uiso 0.50 1 calc PR
H27B H 0.4600 0.5440 0.1092 0.506 Uiso 0.50 1 calc PR
H27C H 0.3870 0.4769 0.1234 0.506 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0027 0.0015 '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 0.0054 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0098 0.0055 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3113 1.3305 '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
O2 Zn1 O2 108.51(5) . 3_565
O2 Zn1 O2 108.51(5) . 2_665
O2 Zn1 O2 108.51(5) 3_565 2_665
O2 Zn1 O1 110.42(5) . .
O2 Zn1 O1 110.42(5) 3_565 .
O2 Zn1 O1 110.42(5) 2_665 .
O2 Zn1 Zn2 75.71(5) . .
O2 Zn1 Zn2 116.74(5) 3_565 .
O2 Zn1 Zn2 130.50(5) 2_665 .
O1 Zn1 Zn2 35.437(9) . .
O2 Zn1 Zn2 116.74(5) . 2_665
O2 Zn1 Zn2 130.50(5) 3_565 2_665
O2 Zn1 Zn2 75.71(5) 2_665 2_665
O1 Zn1 Zn2 35.435(9) . 2_665
Zn2 Zn1 Zn2 60.280(14) . 2_665
O2 Zn1 Zn2 130.50(5) . 3_565
O2 Zn1 Zn2 75.71(5) 3_565 3_565
O2 Zn1 Zn2 116.74(5) 2_665 3_565
O1 Zn1 Zn2 35.435(9) . 3_565
Zn2 Zn1 Zn2 60.281(15) . 3_565
Zn2 Zn1 Zn2 60.278(14) 2_665 3_565
O1 Zn2 O3 112.08(8) . .
O1 Zn2 O5 110.43(5) . 34
O3 Zn2 O5 105.90(7) . 34
O1 Zn2 O4 108.86(6) . 36
O3 Zn2 O4 110.13(7) . 36
O5 Zn2 O4 109.39(7) 34 36
O1 Zn2 Zn1 35.35(7) . .
O3 Zn2 Zn1 77.02(5) . .
O5 Zn2 Zn1 118.02(5) 34 .
O4 Zn2 Zn1 127.96(5) 36 .
C13 N1 C5 119.65(18) . .
C13 N1 C8 120.75(19) . .
C5 N1 C8 117.89(19) . .
Zn1 O1 Zn2 109.21(7) . .
Zn1 O1 Zn2 109.22(7) . 3_565
Zn2 O1 Zn2 109.73(7) . 3_565
Zn1 O1 Zn2 109.22(7) . 2_665
Zn2 O1 Zn2 109.73(7) . 2_665
Zn2 O1 Zn2 109.73(7) 3_565 2_665
C1 O2 Zn1 131.66(15) . .
C1 O3 Zn2 129.35(15) . .
C9 O4 Zn2 128.94(14) . 30_455
C9 O5 Zn2 127.75(14) . 28
O2 C1 O3 125.6(2) . .
O2 C1 C2 116.6(2) . .
O3 C1 C2 117.77(19) . .
C3 C2 C7 119.9(2) . .
C3 C2 C1 120.4(2) . .
C7 C2 C1 119.61(19) . .
C4 C3 C2 119.9(2) . .
C5 C4 C3 120.2(2) . .
C4 C5 C6 119.9(2) . .
C4 C5 N1 120.6(2) . .
C6 C5 N1 119.5(2) . .
C7 C6 C5 119.9(2) . .
C6 C7 C2 119.9(2) . .
O4 C9 O5 124.70(19) . .
O4 C9 C10 117.38(19) . .
O5 C9 C10 117.91(18) . .
C11 C10 C15 118.20(19) . .
C11 C10 C9 120.67(19) . .
C15 C10 C9 121.12(19) . .
C12 C11 C10 121.1(2) . .
C11 C12 C13 121.1(2) . .
N1 C13 C14 120.7(2) . .
N1 C13 C12 121.8(2) . .
C14 C13 C12 117.5(2) . .
C15 C14 C13 120.9(2) . .
C14 C15 C10 121.1(2) . .
C18 C17 C16 111(2) . .
C17 C18 C19 117(2) . .
C20 C19 C18 107.7(18) . .
C21 C20 C19 96(2) . .
C22 C23 C24 116.6(12) . .
C23 C24 C25 115.5(10) . .
C26 C25 C24 117.6(11) . .
C25 C26 C27 116.1(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.9287(15) .
Zn1 O2 1.9288(15) 3_565
Zn1 O2 1.9288(15) 2_665
Zn1 O1 1.934(2) .
Zn1 Zn2 3.1570(6) .
Zn1 Zn2 3.1573(6) 2_665
Zn1 Zn2 3.1573(6) 3_565
Zn2 O1 1.9384(9) .
Zn2 O3 1.9424(15) .
Zn2 O5 1.9431(15) 34
Zn2 O4 1.9484(16) 36
N1 C13 1.387(3) .
N1 C5 1.425(3) .
N1 C8 1.459(3) .
O1 Zn2 1.9385(9) 3_565
O1 Zn2 1.9385(9) 2_665
O2 C1 1.263(3) .
O3 C1 1.267(3) .
O4 C9 1.270(3) .
O4 Zn2 1.9484(15) 30_455
O5 C9 1.276(3) .
O5 Zn2 1.9432(15) 28
C1 C2 1.489(3) .
C2 C3 1.392(3) .
C2 C7 1.397(3) .
C3 C4 1.390(3) .
C4 C5 1.385(3) .
C5 C6 1.399(3) .
C6 C7 1.386(3) .
C9 C10 1.479(3) .
C10 C11 1.390(3) .
C10 C15 1.399(3) .
C11 C12 1.377(3) .
C12 C13 1.409(3) .
C13 C14 1.404(3) .
C14 C15 1.380(3) .
C16 C17 1.58(2) .
C17 C18 1.539(19) .
C18 C19 1.563(18) .
C19 C20 1.559(19) .
C20 C21 1.501(17) .
C22 C23 1.476(16) .
C23 C24 1.500(15) .
C24 C25 1.553(12) .
C25 C26 1.486(13) .
C26 C27 1.529(19) .
