#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:51:12 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257540 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705351.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_7705351
loop_
_publ_author_name
'Menzel, Saskia'
'Millan, Simon'
'H\"ofert, Simon-Patrick'
'Nuhnen, Alexander'
'G\"okpinar, Serkan'
'Schmitz, Alexa'
'Janiak, Christoph'
_publ_section_title
;
Increase of network hydrophilicity from sql to lvt supramolecular isomers
of Cu-MOFs with the bifunctional
4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoate linker.
;
_journal_issue 36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 12854
_journal_page_last 12864
_journal_paper_doi 10.1039/d0dt02642e
_journal_volume 49
_journal_year 2020
_chemical_formula_moiety 'C24 H22 Cu N4 O4, 8.968(H2 O)'
_chemical_formula_sum 'C24 H39.94 Cu N4 O12.96'
_chemical_formula_weight 655.47
_space_group_crystal_system tetragonal
_space_group_IT_number 88
_space_group_name_Hall '-I 4ad'
_space_group_name_H-M_alt 'I 41/a :2'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2017/1
_audit_update_record
;
2020-07-23 deposited with the CCDC. 2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 23.2432(12)
_cell_length_b 23.2432(12)
_cell_length_c 11.9130(7)
_cell_measurement_reflns_used 9155
_cell_measurement_temperature 140(2)
_cell_measurement_theta_max 26.406
_cell_measurement_theta_min 2.478
_cell_volume 6436.0(6)
_computing_cell_refinement 'SAINT (Bruker, 2012)'
_computing_data_collection 'APEX2 (Bruker, 2012)'
_computing_data_reduction 'SAINT (Bruker, 2012)'
_computing_molecular_graphics 'DIAMOND 4.3.1 (Brandenburg, 1999)'
_computing_publication_material 'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution 'SHELXT-2015 (Sheldrick 2015a)'
_diffrn_ambient_temperature 140(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Bruker Kappa APEX-II CCD area detector'
_diffrn_measurement_method '\w scans, \f scans'
_diffrn_radiation_monochromator 'multilayer mirror'
_diffrn_radiation_source 'microfocus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1230
_diffrn_reflns_av_unetI/netI 0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 48071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.473
_diffrn_reflns_theta_min 1.752
_exptl_absorpt_coefficient_mu 0.743
_exptl_absorpt_correction_T_max 0.7454
_exptl_absorpt_correction_T_min 0.6226
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2757
_exptl_crystal_recrystallization_method
'solvent exchange from the methanol-containing structure'
_exptl_crystal_size_max 0.137
_exptl_crystal_size_mid 0.115
_exptl_crystal_size_min 0.059
_refine_diff_density_max 0.705
_refine_diff_density_min -0.478
_refine_diff_density_rms 0.077
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.138
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 236
_refine_ls_number_reflns 3301
_refine_ls_number_restraints 15
_refine_ls_restrained_S_all 1.136
_refine_ls_R_factor_all 0.0420
_refine_ls_R_factor_gt 0.0395
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+15.6649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1088
_refine_ls_wR_factor_ref 0.1103
_reflns_Friedel_coverage 0.000
_reflns_number_gt 3060
_reflns_number_total 3301
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d0dt02642e2.cif
_cod_data_source_block mo_HeeringCHD007H2O_0m
_cod_depositor_comments
'Adding full bibliography for 7705350--7705352.cif.'
_cod_original_cell_volume 6436.0(8)
_cod_original_sg_symbol_H-M 'I 41/a'
_cod_database_code 7705351
_shelx_shelxl_version_number 2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.905
_shelx_estimated_absorpt_t_max 0.957
_shelx_res_file
;
TITL mo_HeeringCHD007H2O_0m in I4(1)/a
mo_HeeringCHD007H2O_0m.res
created by SHELXL-2017/1 at 15:29:30 on 17-Jan-2019
CELL 0.71073 23.2432 23.2432 11.9130 90.000 90.000 90.000
ZERR 8.00 0.0012 0.0012 0.0007 0.000 0.000 0.000
LATT 2
SYMM -y+1/4, x+3/4, z+3/4
SYMM y+1/4, -x+1/4, z+1/4
SYMM -x, -y+1/2, z
SFAC C H O CU N
UNIT 192 319.5 103.7 8 32
LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
TEMP -133.15
SIZE 0.059 0.115 0.137
ACTA
L.S. 5
FMAP 2
PLAN 50
HTAB
BOND $H
CONF
DFIX 0.820000 0.010000 O3 H3A
DFIX 0.820000 0.010000 O3 H3B
DFIX 0.820000 0.010000 O4 H4A
DFIX 0.820000 0.010000 O4 H4B
DFIX 0.820000 0.010000 O5 H5A
DFIX 0.820000 0.010000 O5 H5B
DFIX 0.820000 0.010000 O7 H7A
DFIX 0.820000 0.010000 O7 H7B
DFIX 0.820000 0.010000 O6 H6A
DFIX 0.820000 0.010000 O6 H6B
DANG 1.296731 0.020000 H3A H3B
DANG 1.296731 0.020000 H4A H4B
DANG 1.296731 0.020000 H5A H5B
DANG 1.296731 0.020000 H6A H6B
DANG 1.296731 0.020000 H7A H7B
WGHT 0.045800 15.664901
FVAR 0.19255 0.96305 0.85841 0.90272 0.86337 0.89712
CU1 4 0.000000 0.500000 0.000000 10.50000 0.01334 0.01773 =
0.00835 -0.00584 0.00110 -0.00096
O1 3 0.207728 0.698743 0.650794 11.00000 0.02284 0.01896 =
0.01173 -0.00319 -0.00647 -0.00036
O2 3 0.292650 0.693806 0.567126 11.00000 0.02196 0.02964 =
0.02714 -0.00811 -0.00469 -0.00421
N1 5 0.108071 0.476318 0.107816 11.00000 0.02048 0.01764 =
0.01681 -0.00699 -0.00297 0.00115
H1 2 0.105547 0.445148 0.071196 11.00000 -1.50000
N2 5 0.067345 0.517543 0.096572 11.00000 0.01703 0.01987 =
0.01572 -0.00614 -0.00140 0.00080
C1 1 0.147040 0.489556 0.186720 11.00000 0.02154 0.02127 =
0.01451 -0.00331 -0.00237 -0.00039
C2 1 0.131443 0.542908 0.228801 11.00000 0.02187 0.02085 =
0.01413 -0.00507 -0.00216 -0.00088
C3 1 0.081513 0.559054 0.169112 11.00000 0.02032 0.02018 =
0.01536 -0.00571 -0.00069 -0.00088
C4 1 0.195536 0.450176 0.212468 11.00000 0.03117 0.02560 =
0.02716 -0.00348 -0.00917 0.00590
AFIX 137
H4C 2 0.180654 0.411293 0.225462 11.00000 -1.50000
H4D 2 0.215587 0.463660 0.279882 11.00000 -1.50000
H4E 2 0.222392 0.449570 0.149062 11.00000 -1.50000
AFIX 0
C5 1 0.049710 0.614579 0.174092 11.00000 0.02857 0.02167 =
0.03374 -0.01218 -0.01046 0.00400
AFIX 137
H5C 2 0.029736 0.621029 0.102747 11.00000 -1.50000
H5D 2 0.076908 0.646049 0.187554 11.00000 -1.50000
H5E 2 0.021548 0.613216 0.235255 11.00000 -1.50000
AFIX 0
C6 1 0.160728 0.576549 0.317698 11.00000 0.02324 0.02107 =
0.01587 -0.00494 -0.00518 -0.00078
C7 1 0.128412 0.600398 0.404543 11.00000 0.01890 0.02649 =
0.01958 -0.00655 -0.00245 -0.00089
AFIX 43
H7 2 0.088059 0.594014 0.406885 11.00000 -1.20000
AFIX 0
C8 1 0.154166 0.633256 0.487504 11.00000 0.02110 0.02372 =
0.01646 -0.00652 -0.00053 0.00103
AFIX 43
H8 2 0.131388 0.649314 0.545837 11.00000 -1.20000
AFIX 0
C9 1 0.213303 0.642864 0.485795 11.00000 0.02174 0.01993 =
0.01344 -0.00363 -0.00519 -0.00014
C10 1 0.246129 0.618609 0.400096 11.00000 0.01856 0.03470 =
0.02433 -0.01030 -0.00178 -0.00180
AFIX 43
H10 2 0.286542 0.624655 0.398435 11.00000 -1.20000
AFIX 0
C11 1 0.220231 0.585764 0.317379 11.00000 0.02252 0.03374 =
0.01938 -0.01215 0.00049 0.00048
AFIX 43
H11 2 0.243129 0.569276 0.259686 11.00000 -1.20000
AFIX 0
C12 1 0.240618 0.680668 0.573051 11.00000 0.02187 0.01632 =
0.01590 -0.00011 -0.00744 0.00063
Part 1 21
O3 3 -0.108310 0.350839 0.191804 21.00000 0.02717 0.03250 =
0.05072 0.00513 -0.01067 -0.00719
H3A 2 -0.094298 0.334133 0.138497 21.00000 -1.50000
H3B 2 -0.092407 0.382438 0.190502 21.00000 -1.50000
PART 2 31
O6 3 0.036789 0.389442 0.255778 31.00000 0.03060 0.04249 =
0.05162 0.01852 0.00466 0.00264
H6A 2 0.055480 0.377523 0.202771 31.00000 -1.50000
H6B 2 0.013160 0.412051 0.231137 31.00000 -1.50000
PART 3 41
O7 3 0.515720 0.440254 0.015904 41.00000 0.09584 0.07290 =
0.07635 0.00806 0.00072 -0.00136
H7A 2 0.512110 0.475161 0.008117 41.00000 -1.50000
H7B 2 0.525588 0.436479 0.081957 41.00000 -1.50000
PART 4 51
O5 3 0.001314 0.672645 0.428242 51.00000 0.03763 0.03964 =
0.03489 0.00121 0.00672 0.00533
H5A 2 0.011911 0.690883 0.482987 51.00000 -1.50000
H5B 2 -0.006663 0.640428 0.451020 51.00000 -1.50000
PART 5 61
O4 3 -0.027679 0.303101 0.345938 61.00000 0.03228 0.03132 =
0.04271 0.00783 0.00031 0.00039
H4A 2 -0.005075 0.327357 0.322047 61.00000 -1.50000
H4B 2 -0.016005 0.272572 0.321488 61.00000 -1.50000
PART 0
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM mo_HeeringCHD007H2O_0m in I4(1)/a
REM R1 = 0.0395 for 3060 Fo > 4sig(Fo) and 0.0420 for all 3301 data
REM 236 parameters refined using 15 restraints
END
WGHT 0.0458 15.6650
REM Instructions for potential hydrogen bonds
EQIV $2 -y+3/4, x+1/4, z-3/4
HTAB N1 O1_$2
EQIV $5 y-1/4, -x+1/4, -z+1/4
HTAB N1 O3^a_$5
EQIV $3 y-3/4, -x+3/4, -z+3/4
HTAB O3^a O2_$3
HTAB O6^b O2_$3
EQIV $6 -x+1, -y+1, -z
HTAB O7^c O7^c_$6
EQIV $7 -x, -y+1/2, z
HTAB O4^e O4^e_$7
REM Highest difference peak 0.705, deepest hole -0.478, 1-sigma level 0.077
Q1 1 0.0111 0.3094 0.2167 11.00000 0.05 0.71
Q2 1 -0.0872 0.3322 0.2437 11.00000 0.05 0.59
Q3 1 -0.0336 0.6898 0.3975 11.00000 0.05 0.43
Q4 1 0.0249 0.4072 0.3233 11.00000 0.05 0.42
Q5 1 0.1932 0.5714 0.3377 11.00000 0.05 0.33
Q6 1 -0.0233 0.3139 0.4268 11.00000 0.05 0.29
Q7 1 0.2351 0.4673 0.2069 11.00000 0.05 0.28
Q8 1 0.1806 0.4343 0.2624 11.00000 0.05 0.27
Q9 1 0.0000 0.7500 0.4503 10.50000 0.05 0.26
Q10 1 0.0162 0.4683 0.0349 11.00000 0.05 0.26
Q11 1 0.0000 0.7500 0.3750 10.25000 0.05 0.25
Q12 1 0.4835 0.3973 0.1388 11.00000 0.05 0.25
Q13 1 0.1680 0.4660 0.2113 11.00000 0.05 0.25
Q14 1 0.1951 0.6271 0.5161 11.00000 0.05 0.24
Q15 1 0.2185 0.7254 0.6917 11.00000 0.05 0.24
Q16 1 0.2280 0.6547 0.5302 11.00000 0.05 0.24
Q17 1 0.2300 0.5935 0.3748 11.00000 0.05 0.23
Q18 1 0.1953 0.6863 0.6769 11.00000 0.05 0.23
Q19 1 0.1461 0.5716 0.3716 11.00000 0.05 0.23
Q20 1 0.2760 0.6774 0.5922 11.00000 0.05 0.22
Q21 1 0.0664 0.5816 0.1737 11.00000 0.05 0.22
Q22 1 0.5184 0.4494 -0.0539 11.00000 0.05 0.22
Q23 1 0.2264 0.6753 0.6271 11.00000 0.05 0.21
Q24 1 -0.0973 0.3585 0.1211 11.00000 0.05 0.21
Q25 1 0.0606 0.5261 0.1533 11.00000 0.05 0.20
Q26 1 0.1091 0.5253 0.2540 11.00000 0.05 0.20
Q27 1 0.5066 0.4583 0.1074 11.00000 0.05 0.20
Q28 1 0.1401 0.5139 0.2265 11.00000 0.05 0.20
Q29 1 0.1404 0.5552 0.2755 11.00000 0.05 0.20
Q30 1 0.1012 0.5508 0.2135 11.00000 0.05 0.20
Q31 1 -0.0280 0.6047 0.4931 11.00000 0.05 0.19
Q32 1 0.1637 0.5680 0.1476 11.00000 0.05 0.19
Q33 1 0.3057 0.6607 0.5693 11.00000 0.05 0.19
Q34 1 0.1953 0.4168 0.1715 11.00000 0.05 0.19
Q35 1 0.1134 0.5647 0.1816 11.00000 0.05 0.19
Q36 1 0.0144 0.7232 0.4300 11.00000 0.05 0.18
Q37 1 0.5037 0.4130 -0.0655 11.00000 0.05 0.17
Q38 1 0.1427 0.6238 0.4358 11.00000 0.05 0.17
Q39 1 0.0809 0.5456 0.1308 11.00000 0.05 0.17
Q40 1 0.5618 0.4586 0.0109 11.00000 0.05 0.16
Q41 1 0.0374 0.6924 0.4065 11.00000 0.05 0.16
Q42 1 0.3024 0.7082 0.6653 11.00000 0.05 0.16
Q43 1 0.0989 0.5817 0.4264 11.00000 0.05 0.16
Q44 1 -0.1271 0.3700 0.2277 11.00000 0.05 0.16
Q45 1 0.2479 0.5901 0.2342 11.00000 0.05 0.16
Q46 1 0.0783 0.4758 0.1435 11.00000 0.05 0.16
Q47 1 0.0071 0.6095 -0.0472 11.00000 0.05 0.15
Q48 1 0.5442 0.4230 0.0796 11.00000 0.05 0.15
Q49 1 -0.0319 0.2922 0.1723 11.00000 0.05 0.15
Q50 1 0.0018 0.6579 0.5308 11.00000 0.05 0.15
;
_shelx_res_checksum 30680
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+3/4'
'y+1/4, -x+1/4, z+1/4'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+5/4'
'y+3/4, -x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-3/4'
'-y-1/4, x-1/4, -z-1/4'
'x, y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z-1/4'
'-y+1/4, x+1/4, -z+1/4'
'x+1/2, y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.000000 0.500000 0.000000 0.01314(13) Uani 1 2 d S . P . .
O1 O 0.20773(7) 0.69874(6) 0.65079(12) 0.0178(3) Uani 1 1 d . . . . .
O2 O 0.29265(7) 0.69381(7) 0.56713(14) 0.0262(4) Uani 1 1 d . . . . .
N1 N 0.10807(8) 0.47632(8) 0.10782(15) 0.0183(4) Uani 1 1 d . . . . .
H1 H 0.1055(13) 0.4451(13) 0.071(3) 0.027 Uiso 1 1 d . U . . .
N2 N 0.06734(8) 0.51754(8) 0.09657(15) 0.0175(4) Uani 1 1 d . . . . .
C1 C 0.14704(10) 0.48956(9) 0.18672(18) 0.0191(4) Uani 1 1 d . . . . .
C2 C 0.13144(10) 0.54291(10) 0.22880(18) 0.0190(4) Uani 1 1 d . . . . .
C3 C 0.08151(9) 0.55905(9) 0.16911(18) 0.0186(4) Uani 1 1 d . . . . .
C4 C 0.19554(11) 0.45018(11) 0.2125(2) 0.0280(5) Uani 1 1 d . . . . .
H4C H 0.180654 0.411293 0.225462 0.042 Uiso 1 1 calc R U . . .
H4D H 0.215587 0.463660 0.279882 0.042 Uiso 1 1 calc R U . . .
H4E H 0.222392 0.449570 0.149062 0.042 Uiso 1 1 calc R U . . .
C5 C 0.04971(11) 0.61458(10) 0.1741(2) 0.0280(5) Uani 1 1 d . . . . .
H5C H 0.029736 0.621029 0.102747 0.042 Uiso 1 1 calc R U . . .
H5D H 0.076908 0.646049 0.187554 0.042 Uiso 1 1 calc R U . . .
H5E H 0.021548 0.613216 0.235255 0.042 Uiso 1 1 calc R U . . .
C6 C 0.16073(10) 0.57655(9) 0.31770(18) 0.0201(4) Uani 1 1 d . . . . .
C7 C 0.12841(10) 0.60040(10) 0.40454(19) 0.0217(5) Uani 1 1 d . . . . .
H7 H 0.088059 0.594014 0.406885 0.026 Uiso 1 1 calc R U . . .
C8 C 0.15417(10) 0.63326(10) 0.48750(18) 0.0204(5) Uani 1 1 d . . . . .
H8 H 0.131388 0.649314 0.545837 0.025 Uiso 1 1 calc R U . . .
C9 C 0.21330(10) 0.64286(9) 0.48579(17) 0.0184(4) Uani 1 1 d . . . . .
C10 C 0.24613(10) 0.61861(11) 0.4001(2) 0.0259(5) Uani 1 1 d . . . . .
H10 H 0.286542 0.624655 0.398435 0.031 Uiso 1 1 calc R U . . .
C11 C 0.22023(10) 0.58576(11) 0.31738(19) 0.0252(5) Uani 1 1 d . . . . .
H11 H 0.243129 0.569276 0.259686 0.030 Uiso 1 1 calc R U . . .
C12 C 0.24062(9) 0.68067(9) 0.57305(18) 0.0180(4) Uani 1 1 d . . . . .
O3 O -0.10831(8) 0.35084(9) 0.19180(19) 0.0368(7) Uani 0.963(7) 1 d D . P A 1
H3A H -0.0943(16) 0.3341(13) 0.138(2) 0.055 Uiso 0.963(7) 1 d D U P A 1
H3B H -0.0924(15) 0.3824(8) 0.191(3) 0.055 Uiso 0.963(7) 1 d D U P A 1
O6 O 0.03679(11) 0.38944(11) 0.2558(2) 0.0416(9) Uani 0.858(8) 1 d D . P B 2
H6A H 0.0555(17) 0.3775(19) 0.203(2) 0.062 Uiso 0.858(8) 1 d D U P B 2
H6B H 0.0132(15) 0.4121(16) 0.231(3) 0.062 Uiso 0.858(8) 1 d D U P B 2
O7 O 0.5157(2) 0.44025(17) 0.0159(3) 0.0817(15) Uani 0.903(10) 1 d D . P C 3
H7A H 0.512(3) 0.4752(7) 0.008(5) 0.123 Uiso 0.903(10) 1 d D U P C 3
H7B H 0.526(3) 0.436(3) 0.082(2) 0.123 Uiso 0.903(10) 1 d D U P C 3
O5 O 0.00131(10) 0.67265(11) 0.42824(19) 0.0374(8) Uani 0.863(8) 1 d D . P D 4
H5A H 0.012(2) 0.6909(14) 0.483(2) 0.056 Uiso 0.863(8) 1 d D U P D 4
H5B H -0.0067(19) 0.6404(8) 0.451(3) 0.056 Uiso 0.863(8) 1 d D U P D 4
O4 O -0.02768(9) 0.30310(10) 0.34594(19) 0.0354(8) Uani 0.897(8) 1 d D . P E 5
H4A H -0.0051(14) 0.3274(11) 0.322(3) 0.053 Uiso 0.897(8) 1 d D U P E 5
H4B H -0.0160(16) 0.2726(8) 0.321(3) 0.053 Uiso 0.897(8) 1 d D U P E 5
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.01334(19) 0.0177(2) 0.00835(19) -0.00584(12) 0.00110(12) -0.00096(13)
O1 0.0228(8) 0.0190(7) 0.0117(7) -0.0032(6) -0.0065(6) -0.0004(6)
O2 0.0220(8) 0.0296(9) 0.0271(9) -0.0081(7) -0.0047(7) -0.0042(7)
N1 0.0205(9) 0.0176(9) 0.0168(9) -0.0070(7) -0.0030(7) 0.0011(7)
N2 0.0170(9) 0.0199(9) 0.0157(8) -0.0061(7) -0.0014(7) 0.0008(7)
C1 0.0215(10) 0.0213(10) 0.0145(10) -0.0033(8) -0.0024(8) -0.0004(8)
C2 0.0219(11) 0.0209(11) 0.0141(9) -0.0051(8) -0.0022(8) -0.0009(8)
C3 0.0203(10) 0.0202(10) 0.0154(10) -0.0057(8) -0.0007(8) -0.0009(8)
C4 0.0312(13) 0.0256(12) 0.0272(12) -0.0035(10) -0.0092(10) 0.0059(10)
C5 0.0286(12) 0.0217(11) 0.0337(13) -0.0122(10) -0.0105(10) 0.0040(9)
C6 0.0232(11) 0.0211(10) 0.0159(10) -0.0049(8) -0.0052(8) -0.0008(9)
C7 0.0189(10) 0.0265(11) 0.0196(11) -0.0066(9) -0.0024(8) -0.0009(9)
C8 0.0211(11) 0.0237(11) 0.0165(10) -0.0065(8) -0.0005(8) 0.0010(9)
C9 0.0217(11) 0.0199(10) 0.0134(10) -0.0036(8) -0.0052(8) -0.0001(8)
C10 0.0186(11) 0.0347(13) 0.0243(12) -0.0103(10) -0.0018(9) -0.0018(9)
C11 0.0225(11) 0.0337(13) 0.0194(11) -0.0122(9) 0.0005(9) 0.0005(10)
C12 0.0219(10) 0.0163(10) 0.0159(10) -0.0001(8) -0.0074(8) 0.0006(8)
O3 0.0272(11) 0.0325(11) 0.0507(14) 0.0051(9) -0.0107(9) -0.0072(8)
O6 0.0306(14) 0.0425(16) 0.0516(17) 0.0185(11) 0.0047(10) 0.0026(10)
O7 0.096(3) 0.073(2) 0.076(2) 0.0081(18) 0.001(2) -0.001(2)
O5 0.0376(14) 0.0396(14) 0.0349(13) 0.0012(10) 0.0067(10) 0.0053(10)
O4 0.0323(12) 0.0313(12) 0.0427(14) 0.0078(9) 0.0003(9) 0.0004(9)
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'
N N 0.0061 0.0033 '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 O1 180.00(8) 14_466 6_543 ?
O1 Cu1 N2 88.45(7) 14_466 9_565 ?
O1 Cu1 N2 91.55(7) 6_543 9_565 ?
O1 Cu1 N2 91.55(7) 14_466 . ?
O1 Cu1 N2 88.45(7) 6_543 . ?
N2 Cu1 N2 180.0 9_565 . ?
C12 O1 Cu1 109.95(13) . 7_455 ?
C1 N1 N2 112.29(18) . . ?
C1 N1 H1 127(2) . . ?
N2 N1 H1 120(2) . . ?
C3 N2 N1 105.95(17) . . ?
C3 N2 Cu1 135.84(15) . . ?
N1 N2 Cu1 117.61(13) . . ?
N1 C1 C2 106.39(19) . . ?
N1 C1 C4 121.1(2) . . ?
C2 C1 C4 132.5(2) . . ?
C1 C2 C3 105.71(18) . . ?
C1 C2 C6 127.6(2) . . ?
C3 C2 C6 126.7(2) . . ?
N2 C3 C2 109.65(19) . . ?
N2 C3 C5 122.0(2) . . ?
C2 C3 C5 128.22(19) . . ?
C1 C4 H4C 109.5 . . ?
C1 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
C1 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
C3 C5 H5C 109.5 . . ?
C3 C5 H5D 109.5 . . ?
H5C C5 H5D 109.5 . . ?
C3 C5 H5E 109.5 . . ?
H5C C5 H5E 109.5 . . ?
H5D C5 H5E 109.5 . . ?
C7 C6 C11 118.3(2) . . ?
C7 C6 C2 119.5(2) . . ?
C11 C6 C2 122.2(2) . . ?
C8 C7 C6 121.1(2) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 120.3(2) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 119.09(19) . . ?
C8 C9 C12 120.06(19) . . ?
C10 C9 C12 120.8(2) . . ?
C11 C10 C9 120.4(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C6 120.8(2) . . ?
C10 C11 H11 119.6 . . ?
C6 C11 H11 119.6 . . ?
O2 C12 O1 122.82(19) . . ?
O2 C12 C9 120.9(2) . . ?
O1 C12 C9 116.30(19) . . ?
H3A O3 H3B 103(2) . . ?
H6A O6 H6B 107(2) . . ?
H7A O7 H7B 104(3) . . ?
H5A O5 H5B 106(2) . . ?
H4A O4 H4B 105(2) . . ?
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 1.9446(14) 14_466 ?
Cu1 O1 1.9446(14) 6_543 ?
Cu1 N2 1.9849(17) 9_565 ?
Cu1 N2 1.9850(17) . ?
O1 C12 1.272(3) . ?
O2 C12 1.249(3) . ?
N1 C1 1.341(3) . ?
N1 N2 1.354(3) . ?
N1 H1 0.85(3) . ?
N2 C3 1.336(3) . ?
C1 C2 1.386(3) . ?
C1 C4 1.484(3) . ?
C2 C3 1.412(3) . ?
C2 C6 1.482(3) . ?
C3 C5 1.488(3) . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
C5 H5C 0.9800 . ?
C5 H5D 0.9800 . ?
C5 H5E 0.9800 . ?
C6 C7 1.393(3) . ?
C6 C11 1.400(3) . ?
C7 C8 1.385(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.394(3) . ?
C9 C12 1.502(3) . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
O3 H3A 0.812(10) . ?
O3 H3B 0.822(10) . ?
O6 H6A 0.815(10) . ?
O6 H6B 0.815(10) . ?
O7 H7A 0.821(10) . ?
O7 H7B 0.824(10) . ?
O5 H5A 0.816(10) . ?
O5 H5B 0.818(10) . ?
O4 H4A 0.822(10) . ?
O4 H4B 0.814(10) . ?
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
N1 H1 O1 0.85(3) 2.41(3) 2.831(2) 111(2) 6_543
N1 H1 O3 0.85(3) 2.03(3) 2.811(3) 153(3) 10_566
O3 H3B O2 0.822(10) 1.936(11) 2.758(3) 178(4) 14_466
O6 H6B O2 0.815(10) 2.009(14) 2.814(3) 169(5) 14_466
O7 H7A O7 0.821(10) 2.09(2) 2.897(8) 168(8) 9_665
O4 H4B O4 0.814(10) 2.05(2) 2.784(4) 150(4) 4
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C3 1.3(2) . . . . ?
C1 N1 N2 Cu1 -171.16(15) . . . . ?
N2 N1 C1 C2 -0.8(3) . . . . ?
N2 N1 C1 C4 -179.9(2) . . . . ?
N1 C1 C2 C3 -0.1(2) . . . . ?
C4 C1 C2 C3 178.9(2) . . . . ?
N1 C1 C2 C6 -179.9(2) . . . . ?
C4 C1 C2 C6 -0.9(4) . . . . ?
N1 N2 C3 C2 -1.3(2) . . . . ?
Cu1 N2 C3 C2 169.10(17) . . . . ?
N1 N2 C3 C5 174.3(2) . . . . ?
Cu1 N2 C3 C5 -15.3(4) . . . . ?
C1 C2 C3 N2 0.9(3) . . . . ?
C6 C2 C3 N2 -179.2(2) . . . . ?
C1 C2 C3 C5 -174.4(2) . . . . ?
C6 C2 C3 C5 5.5(4) . . . . ?
C1 C2 C6 C7 -132.4(3) . . . . ?
C3 C2 C6 C7 47.8(3) . . . . ?
C1 C2 C6 C11 48.1(4) . . . . ?
C3 C2 C6 C11 -131.8(3) . . . . ?
C11 C6 C7 C8 1.1(4) . . . . ?
C2 C6 C7 C8 -178.4(2) . . . . ?
C6 C7 C8 C9 -0.3(4) . . . . ?
C7 C8 C9 C10 -0.5(3) . . . . ?
C7 C8 C9 C12 177.3(2) . . . . ?
C8 C9 C10 C11 0.5(4) . . . . ?
C12 C9 C10 C11 -177.3(2) . . . . ?
C9 C10 C11 C6 0.4(4) . . . . ?
C7 C6 C11 C10 -1.2(4) . . . . ?
C2 C6 C11 C10 178.4(2) . . . . ?
Cu1 O1 C12 O2 2.0(3) 7_455 . . . ?
Cu1 O1 C12 C9 -176.93(14) 7_455 . . . ?
C8 C9 C12 O2 -173.7(2) . . . . ?
C10 C9 C12 O2 4.1(3) . . . . ?
C8 C9 C12 O1 5.3(3) . . . . ?
C10 C9 C12 O1 -176.9(2) . . . . ?