#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/41/1514158.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_1514158
loop_
_publ_author_name
'McKellar, Scott C.'
'Graham, Alexander J.'
'Allan, David R.'
'Mohideen, M Infas H'
'Morris, Russell E.'
'Moggach, Stephen A.'
_publ_section_title
;
 The effect of pressure on the post-synthetic modification of a nanoporous
 metal-organic framework.
;
_journal_issue                   8
_journal_name_full               Nanoscale
_journal_page_first              4163
_journal_page_last               4173
_journal_paper_doi               10.1039/c3nr04161a
_journal_volume                  6
_journal_year                    2014
_chemical_formula_moiety         'C32.00 H25.00 Cu3 N1.00 O20.00.2.5(CH3CN)'
_chemical_formula_sum            'C37 H32.5 Cu3 N3.5 O20'
_chemical_formula_weight         1036.805
_space_group_IT_number           164
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"'
_symmetry_space_group_name_H-M   'P -3 m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-05-10
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.5488(13)
_cell_length_b                   18.5488(13)
_cell_length_c                   6.9375(4)
_cell_measurement_reflns_used    1372
_cell_measurement_temperature    298
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     2067.1(2)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         0.3
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.769
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6642
_diffrn_reflns_theta_full        15.612
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         3.199
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.62
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1052.00
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
see above for details 
;
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9979
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         449
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.0001632
_refine_ls_shift/su_mean         0.0000079
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.723 0.165 0.128 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0994
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0654
_reflns_limit_h_max              0
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              0
_reflns_number_gt                449
_reflns_number_total             626
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.60
_oxford_diffrn_Wilson_scale      129.17
_oxford_refine_ls_r_factor_ref   0.0558
_oxford_refine_ls_scale          0.1364(10)
_oxford_reflns_number_all        608
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'st2016 in P-3m1'
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           ST1009
_cod_original_sg_symbol_Hall     '-P 3 2'
_cod_original_sg_symbol_H-M      'P -3 m 1 '
_cod_original_formula_sum        'C37 H32.50 Cu3 N3.50 O20.00'
_cod_database_code               1514158
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT N    (    1 ,X'S,U[ISO]) 
CONT O    (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U[ISO]) 
CONT O    (    4 ,X'S,U'S)  UNTIL C    (    7 ) 
CONT C    (    8 ,X'S,U[ISO])  UNTIL C    (    9 ) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
DISTANCE 1.450000 , 0.050000 = C(9) TO C(8) 
DISTANCE 1.130000 , 0.050000 = N(1) TO C(8) 
DISTANCE 2.180000 , 0.050000 = CU(1) TO N(1) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
ANGLE 170.000000 , 1.000000 = CU(1) TO N(1) TO C(8) 
ANGLE 90.000000 , 1.000000 = N(1) TO CU(1) TO O(1) 
ANGLE 180.000000 , 1.000000 = N(1) TO C(8) TO C(9) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(92) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(91) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00500 = O(3) TO N(1) 
VIBR .0, 0.00500 = O(1) TO N(1) 
VIBR .0, 0.00500 = O(1) TO O(3) 
VIBR .0, 0.00200 = N(1) TO C(8) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(5) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00500 = O(4) TO C(4) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = C(9) TO C(8) 
VIBR .0, 0.00500 = N(1) TO C(9) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = N(1) TO C(8) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO O(4,4,1,1) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
U(IJ) .0, 0.08000 = C(9) TO C(8) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 0.950000 , 0.050000 = C(9) TO H(91) 
DISTANCE 0.950000 , 0.050000 = C(9) TO H(92) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
END                                                                             
;
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x-y,x,-z
-x+y,-x,z
-x,-x+y,-z
x,x-y,z
-x+y,y,z
x-y,-y,-z
y,x,-z
-y,-x,z
y,-x+y,-z
-y,x-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.47614(7) 0.52386(7) 0.8474(3) 0.0257 1.0000 Uani DS T
N1 N 0.4321(10) 0.5679(10) 0.607(4) 0.044(4) 0.3330 Uiso DS U
O1 O 0.5883(5) 0.5601(6) 0.7516(10) 0.0435 1.0000 Uani D U
O2 O 0.6288(5) 0.5179(6) 1.0131(10) 0.0420 1.0000 Uani . U
O3 O 0.4425(6) 0.5575(6) 0.582(2) 0.042(4) 0.6670 Uiso S U
O4 O 0.7922(7) 0.7049(8) 0.2350(14) 0.0883 1.0000 Uani . U
C1 C 0.6420(8) 0.5507(8) 0.8469(16) 0.0355 1.0000 Uani . U
C2 C 0.7241(8) 0.5773(9) 0.7562(14) 0.0348 1.0000 Uani D U
C3 C 0.7427(8) 0.6151(8) 0.5801(15) 0.0330 1.0000 Uani D U
C4 C 0.8188(6) 0.6377(13) 0.493(2) 0.0423 1.0000 Uani DS TU
C5 C 0.7787(6) 0.5573(12) 0.845(2) 0.0294 1.0000 Uani DS TU
C6 C 0.8409(7) 0.6819(15) 0.302(3) 0.0579 1.0000 Uani S TU
C7 C 0.8036(15) 0.7524(17) 0.076(3) 0.1008 0.5000 Uani D U
C8 C 0.4022(10) 0.5978(10) 0.510(4) 0.045(4) 0.3330 Uiso DS U
C9 C 0.3628(5) 0.6372(5) 0.397(3) 0.045(5) 0.3330 Uiso DS U
H31 H 0.7078 0.6333 0.5228 0.0500 1.0000 Uiso . .
H51 H 0.7656 0.5312 0.9706 0.0500 1.0000 Uiso . .
H91 H 0.3680 0.6320 0.2540 0.0475 0.3330 Uiso D .
H92 H 0.3045 0.6091 0.4285 0.0475 0.6670 Uiso D .
H101 H 0.4604 0.5961 0.5838 0.0500 0.6670 Uiso . .
H71 H 0.7571 0.7609 0.0568 0.1172 0.5000 Uiso D .
H72 H 0.8526 0.8064 0.0897 0.1172 0.5000 Uiso D .
H73 H 0.8101 0.7270 -0.0374 0.1172 0.5000 Uiso D .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 10_665 Cu1 O2 2_667 90.1(4) yes
O1 10_665 Cu1 O2 9_557 169.3(3) yes
O2 2_667 Cu1 O2 9_557 88.2(5) yes
O1 10_665 Cu1 Cu1 2_667 84.8(2) yes
O2 2_667 Cu1 Cu1 2_667 84.5(2) yes
O2 9_557 Cu1 Cu1 2_667 84.5(2) yes
O1 10_665 Cu1 N1 . 98.3(5) yes
O2 2_667 Cu1 N1 . 92.3(5) yes
O2 9_557 Cu1 N1 . 92.3(5) yes
Cu1 2_667 Cu1 N1 . 175.6(6) yes
O1 10_665 Cu1 O1 . 89.5(5) yes
O2 2_667 Cu1 O1 . 169.3(3) yes
O2 9_557 Cu1 O1 . 90.1(4) yes
Cu1 2_667 Cu1 O1 . 84.8(2) yes
N1 . Cu1 O1 . 98.3(5) yes
O1 10_665 Cu1 O3 . 91.2(4) yes
O2 2_667 Cu1 O3 . 99.5(4) yes
O2 9_557 Cu1 O3 . 99.5(4) yes
Cu1 2_667 Cu1 O3 . 174.5(5) yes
N1 . Cu1 O3 . 10.0(8) yes
O1 . Cu1 O3 . 91.2(4) yes
Cu1 . N1 C8 . 165.5(9) yes
Cu1 . O1 C1 . 123.0(7) yes
Cu1 2_667 O2 C1 . 123.7(8) yes
Cu1 . O3 H101 10_665 104.5 no
Cu1 . O3 H101 . 104.5 no
H101 10_665 O3 H101 . 115.1 no
C6 . O4 C7 . 127.6(16) yes
O1 . C1 O2 . 123.9(11) yes
O1 . C1 C2 . 118.4(10) yes
O2 . C1 C2 . 117.7(12) yes
C1 . C2 C3 . 120.3(11) yes
C1 . C2 C5 . 119.2(10) yes
C3 . C2 C5 . 120.3(12) yes
C2 . C3 C4 . 120.1(12) yes
C2 . C3 H31 . 120.8 no
C4 . C3 H31 . 118.5 no
C3 7_655 C4 C3 . 119.3(15) yes
C3 7_655 C4 C6 . 120.3(7) yes
C3 . C4 C6 . 120.3(7) yes
C2 . C5 C2 7_655 119.8(14) yes
C2 . C5 H51 . 120.1 no
C2 7_655 C5 H51 . 120.1 no
C4 . C6 O4 . 117.5(9) yes
C4 . C6 O4 7_655 117.5(9) yes
O4 . C6 O4 7_655 124.1(19) yes
H71 9_555 C7 O4 . 138.3 no
H71 9_555 C7 H71 . 39.7 no
O4 . C7 H71 . 111.1 no
H71 9_555 C7 H72 . 107.4 no
O4 . C7 H72 . 111.0 no
H71 . C7 H72 . 107.4 no
H71 9_555 C7 H73 . 70.3 no
O4 . C7 H73 . 111.5 no
H71 . C7 H73 . 107.9 no
H72 . C7 H73 . 107.8 no
N1 . C8 C9 . 176.4(9) yes
C8 . C9 C9 4_565 137.5(4) yes
C8 . C9 C9 6_565 137.5(4) yes
C9 4_565 C9 C9 6_565 60.000(3) yes
C8 . C9 H92 10_665 108.1 no
C9 4_565 C9 H92 10_665 89.0 no
C9 6_565 C9 H92 10_665 31.5 no
C8 . C9 H91 . 112.0 no
C9 4_565 C9 H91 . 98.3 no
C9 6_565 C9 H91 . 98.3 no
H92 10_665 C9 H91 . 107.8 no
C8 . C9 H92 . 108.1 no
C9 4_565 C9 H92 . 31.5 no
C9 6_565 C9 H92 . 89.0 no
H92 10_665 C9 H92 . 113.2 no
H91 . C9 H92 . 107.8 no
C9 4_565 H92 C9 . 117.1 no
C7 . H71 C7 9_555 124.2 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O1 10_665 1.955(9) yes
Cu1 O2 2_667 1.954(8) yes
Cu1 O2 9_557 1.954(8) yes
Cu1 Cu1 2_667 2.614(4) yes
Cu1 N1 . 2.19(4) yes
Cu1 O1 . 1.955(9) yes
Cu1 O3 . 2.137(19) yes
N1 C8 . 1.17(4) yes
O1 C1 . 1.279(14) yes
O2 C1 . 1.270(13) yes
O3 H101 10_665 0.621 no
O3 H101 . 0.621 no
O4 C6 . 1.265(12) yes
O4 C7 . 1.36(3) yes
C1 C2 . 1.485(17) yes
C2 C3 . 1.363(14) yes
C2 C5 . 1.384(13) yes
C3 C4 . 1.394(13) yes
C3 H31 . 0.955 no
C4 C6 . 1.51(3) yes
C5 H51 . 0.968 no
C7 H71 9_555 1.248 no
C7 H71 . 0.962 no
C7 H72 . 0.962 no
C7 H73 . 0.957 no
C8 C9 . 1.49(4) yes
C9 C9 4_565 1.64(3) yes
C9 C9 6_565 1.64(3) yes
C9 H92 10_665 0.960 no
C9 H91 . 1.009 no
C9 H92 . 0.960 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C9 . H92 C8 4_565 157.0(11) 0.960 2.007 2.91(2) yes
C9 4_565 H92 C8 . 157.0(11) 0.960 2.007 2.91(2) yes
C7 . H71 O4 9_555 130.8(14) 0.962 2.436 3.15(2) yes
C7 . H71 C7 9_555 124(2) 0.962 1.248 1.96(2) yes
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 0.000 0.000 -0.065 249 68 ' '
2 0.333 0.667 -0.125 54 25 ' '
3 0.667 0.333 0.125 54 25 ' '
#BEGIN Loops that were not found in dictionaries:
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
-11 15 1 x
-2 12 0 x
-11 14 1 x
-12 17 2 x
-12 15 1 x
0 9 4 x
-11 13 2 x
-11 16 2 x
-8 17 2 x
-6 14 1 x
-4 15 2 x
-10 11 5 x
-4 8 1 x
#END Loops that were not found in dictionaries
