#------------------------------------------------------------------------------
#$Date: 2017-04-29 04:09:08 +0300 (Sat, 29 Apr 2017) $
#$Revision: 195855 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/00/7120048.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_7120048
loop_
_publ_author_name
'Barbour, Len'
'Bezuidenhout, Charl Xavier'
'Esterhuysen, Catharine'
_publ_section_title
;
 Solvatochromism as a probe to observe the solvent exchange process in a
 1-D porous coordination polymer with 1-D solvent accessible channels.
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02492D
_journal_year                    2017
_chemical_formula_moiety         'C10 H10 Cu N3 O4, C H Cl3'
_chemical_formula_sum            'C11 H11 Cl3 Cu N3 O4'
_chemical_formula_weight         419.12
_chemical_name_systematic        Cu(OAc)2Dptz.(Chloroform)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-03-31 deposited with the CCDC.
2017-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                97.495(2)
_cell_angle_beta                 101.910(2)
_cell_angle_gamma                97.661(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2492(11)
_cell_length_b                   8.0459(12)
_cell_length_c                   13.881(2)
_cell_measurement_reflns_used    4724
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.59
_cell_volume                     774.6(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9040
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0822 before and 0.0312 after correction.
The Ratio of minimum to maximum transmission is 0.8292.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.654
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0239
_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)+(0.0254P)²+0.3694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                3252
_reflns_number_total             3586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc02492d11.cif
_cod_data_source_block           solve1
_cod_database_code               7120048
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Cl(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl1A(0.449) Cl2A(0.449) Cl3A(0.449) Cl1B(0.551) Cl2B(0.551)
 Cl3B(0.551)
3.a Aromatic/amide H refined with riding coordinates:
 C51(H51), C41(H41), C21(H21), C11(H11)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_olex2_submission_original_sample_id cxb_CuOAcBptz_CF
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Cu1 Cu 0.63307(3) 0.57735(2) 0.576458(14) 0.00840(6) Uani 1 d . . .
O1 O 0.48871(16) 0.76824(15) 0.57373(9) 0.0134(2) Uani 1 d . . .
O2 O 0.47048(17) 0.47991(15) 0.65969(9) 0.0143(3) Uani 1 d . . .
O3 O 0.73550(17) 0.36256(15) 0.56126(9) 0.0154(3) Uani 1 d . . .
O4 O 0.75769(17) 0.65402(16) 0.47273(9) 0.0144(3) Uani 1 d . . .
N11 N 0.87238(19) 0.69504(17) 0.69815(10) 0.0102(3) Uani 1 d . . .
N21 N 1.5269(2) 0.88889(19) 0.92290(10) 0.0129(3) Uani 1 d . . .
N31 N 1.3240(2) 1.03798(19) 1.00460(11) 0.0138(3) Uani 1 d . . .
C1 C 0.3393(2) 0.7630(2) 0.50708(13) 0.0116(3) Uani 1 d . . .
C2 C 0.2421(3) 0.9168(2) 0.50806(14) 0.0165(4) Uani 1 d . . .
H2A H 0.2986 0.9963 0.5702 0.025 Uiso 1 calc . . GR
H2B H 0.1055 0.8819 0.5036 0.025 Uiso 1 calc . . GR
H2C H 0.2590 0.9725 0.4510 0.025 Uiso 1 calc . . GR
C3 C 0.3110(2) 0.3863(2) 0.61987(13) 0.0121(3) Uani 1 d . . .
C4 C 0.1944(3) 0.3172(2) 0.68825(13) 0.0174(4) Uani 1 d . . .
H4A H 0.0590 0.3204 0.6616 0.026 Uiso 1 calc . . GR
H4B H 0.2365 0.3867 0.7547 0.026 Uiso 1 calc . . GR
H4C H 0.2119 0.1996 0.6929 0.026 Uiso 1 calc . . GR
C51 C 1.0501(2) 0.7025(2) 0.68369(12) 0.0128(3) Uani 1 d . . .
H51 H 1.0661 0.6546 0.6203 0.015 Uiso 1 calc . . R
C41 C 1.2114(2) 0.7763(2) 0.75640(13) 0.0137(3) Uani 1 d . . .
H41 H 1.3352 0.7784 0.7433 0.016 Uiso 1 calc . . R
C31 C 1.1882(2) 0.8474(2) 0.84928(12) 0.0105(3) Uani 1 d . . .
C21 C 1.0043(2) 0.8396(2) 0.86522(13) 0.0132(3) Uani 1 d . . .
H21 H 0.9839 0.8865 0.9279 0.016 Uiso 1 calc . . R
C11 C 0.8518(2) 0.7624(2) 0.78819(13) 0.0128(3) Uani 1 d . . .
H11 H 0.7264 0.7567 0.7995 0.015 Uiso 1 calc . . R
C61 C 1.3552(2) 0.9293(2) 0.92984(12) 0.0110(3) Uani 1 d . . .
C5 C 0.7321(3) 0.3194(3) 0.82336(15) 0.0247(4) Uani 1 d . . .
Cl1A Cl 0.6315(17) 0.1168(16) 0.7454(12) 0.0199(12) Uani 0.45 d A 1 .
Cl2A Cl 0.9649(17) 0.3433(11) 0.8896(10) 0.0402(16) Uani 0.45 d A 1 .
Cl3A Cl 0.586(2) 0.363(2) 0.9122(11) 0.0261(9) Uani 0.45 d A 1 .
Cl1B Cl 0.6401(15) 0.1220(15) 0.7530(11) 0.032(2) Uani 0.55 d A 2 .
H5 H 0.731(3) 0.403(3) 0.7784(19) 0.039 Uiso 1 d . . R
Cl2B Cl 0.9708(13) 0.3046(9) 0.8865(8) 0.0298(8) Uani 0.55 d A 2 .
Cl3B Cl 0.5991(19) 0.3787(17) 0.9076(9) 0.034(2) Uani 0.55 d A 2 .
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'
N N 0.0061 0.0033 '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
O1 Cu1 Cu1 86.03(4) . 2_666
O1 Cu1 O2 88.19(5) . .
O1 Cu1 O3 169.43(5) . .
O1 Cu1 O4 90.81(5) . .
O1 Cu1 N11 98.13(5) . .
O2 Cu1 Cu1 86.48(4) . 2_666
O2 Cu1 O3 89.23(5) . .
O2 Cu1 N11 96.42(5) . .
O3 Cu1 Cu1 83.58(4) . 2_666
O3 Cu1 N11 92.35(5) . .
O4 Cu1 Cu1 83.13(4) . 2_666
O4 Cu1 O2 169.61(5) . .
O4 Cu1 O3 89.89(5) . .
O4 Cu1 N11 93.96(5) . .
N11 Cu1 Cu1 174.98(4) . 2_666
C1 O1 Cu1 121.40(11) . .
C3 O2 Cu1 120.65(11) . .
C1 O3 Cu1 124.00(11) 2_666 .
C3 O4 Cu1 124.69(11) 2_666 .
C51 N11 Cu1 119.09(11) . .
C51 N11 C11 117.77(14) . .
C11 N11 Cu1 123.14(11) . .
N31 N21 C61 117.33(14) 2_877 .
N21 N31 C61 117.73(14) 2_877 .
O1 C1 O3 124.91(15) . 2_666
O1 C1 C2 117.97(15) . .
O3 C1 C2 117.12(15) 2_666 .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O2 C3 C4 117.59(15) . .
O4 C3 O2 125.05(16) 2_666 .
O4 C3 C4 117.36(15) 2_666 .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4B 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N11 C51 H51 118.3 . .
N11 C51 C41 123.30(15) . .
C41 C51 H51 118.3 . .
C51 C41 H41 120.8 . .
C51 C41 C31 118.44(15) . .
C31 C41 H41 120.8 . .
C41 C31 C61 120.98(15) . .
C21 C31 C41 118.70(15) . .
C21 C31 C61 120.32(15) . .
C31 C21 H21 120.6 . .
C11 C21 C31 118.71(15) . .
C11 C21 H21 120.6 . .
N11 C11 C21 123.07(15) . .
N11 C11 H11 118.5 . .
C21 C11 H11 118.5 . .
N21 C61 C31 117.53(14) . .
N31 C61 N21 124.94(15) . .
N31 C61 C31 117.53(15) . .
Cl1A C5 Cl3A 109.1(6) . .
Cl1A C5 H5 106.0(15) . .
Cl2A C5 Cl1A 117.1(5) . .
Cl2A C5 Cl3A 107.6(6) . .
Cl2A C5 Cl1B 115.4(5) . .
Cl2A C5 H5 105.6(15) . .
Cl2A C5 Cl2B 10.1(5) . .
Cl2A C5 Cl3B 106.8(6) . .
Cl3A C5 H5 111.5(16) . .
Cl1B C5 Cl1A 2.4(9) . .
Cl1B C5 Cl3A 108.6(7) . .
Cl1B C5 H5 108.3(16) . .
Cl1B C5 Cl2B 105.5(5) . .
Cl1B C5 Cl3B 112.8(6) . .
Cl2B C5 Cl1A 107.3(5) . .
Cl2B C5 Cl3A 110.9(6) . .
Cl2B C5 H5 111.9(15) . .
Cl3B C5 Cl1A 113.3(6) . .
Cl3B C5 Cl3A 4.8(11) . .
Cl3B C5 H5 107.5(15) . .
Cl3B C5 Cl2B 110.9(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu1 2.5994(5) 2_666
Cu1 O1 1.9705(12) .
Cu1 O2 1.9724(12) .
Cu1 O3 1.9733(12) .
Cu1 O4 1.9723(12) .
Cu1 N11 2.1668(14) .
O1 C1 1.263(2) .
O2 C3 1.267(2) .
O3 C1 1.267(2) 2_666
O4 C3 1.261(2) 2_666
N11 C51 1.339(2) .
N11 C11 1.342(2) .
N21 N31 1.3242(19) 2_877
N21 C61 1.347(2) .
N31 N21 1.3242(19) 2_877
N31 C61 1.344(2) .
C1 O3 1.267(2) 2_666
C1 C2 1.503(2) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 O4 1.261(2) 2_666
C3 C4 1.506(2) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C51 H51 0.9500 .
C51 C41 1.382(2) .
C41 H41 0.9500 .
C41 C31 1.393(2) .
C31 C21 1.391(2) .
C31 C61 1.478(2) .
C21 H21 0.9500 .
C21 C11 1.381(2) .
C11 H11 0.9500 .
C5 Cl1A 1.804(15) .
C5 Cl2A 1.720(13) .
C5 Cl3A 1.816(15) .
C5 Cl1B 1.722(13) .
C5 H5 0.98(3) .
C5 Cl2B 1.798(10) .
C5 Cl3B 1.722(12) .
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_4
Cu1 Cu1 O1 C1 -2.72(12) 2_666 .
Cu1 Cu1 O2 C3 0.00(12) 2_666 .
Cu1 Cu1 O3 C1 1.96(13) 2_666 2_666
Cu1 Cu1 O4 C3 -0.68(13) 2_666 2_666
Cu1 Cu1 N11 C51 20.5(5) 2_666 .
Cu1 Cu1 N11 C11 -159.8(4) 2_666 .
Cu1 O1 C1 O3 2.2(2) . 2_666
Cu1 O1 C1 C2 -177.62(11) . .
Cu1 O2 C3 O4 0.5(2) . 2_666
Cu1 O2 C3 C4 -179.73(11) . .
Cu1 N11 C51 C41 179.39(13) . .
Cu1 N11 C11 C21 -179.00(13) . .
O1 Cu1 O2 C3 86.13(13) . .
O1 Cu1 O3 C1 12.6(4) . 2_666
O1 Cu1 O4 C3 -86.58(13) . 2_666
O1 Cu1 N11 C51 -125.21(13) . .
O1 Cu1 N11 C11 54.49(14) . .
O2 Cu1 O1 C1 -89.32(13) . .
O2 Cu1 O3 C1 88.50(14) . 2_666
O2 Cu1 O4 C3 -2.2(4) . 2_666
O2 Cu1 N11 C51 145.71(13) . .
O2 Cu1 N11 C11 -34.60(14) . .
O3 Cu1 O1 C1 -13.4(4) . .
O3 Cu1 O2 C3 -83.62(13) . .
O3 Cu1 O4 C3 82.87(13) . 2_666
O3 Cu1 N11 C51 56.23(13) . .
O3 Cu1 N11 C11 -124.08(13) . .
O4 Cu1 O1 C1 80.34(13) . .
O4 Cu1 O2 C3 1.5(4) . .
O4 Cu1 O3 C1 -81.14(14) . 2_666
O4 Cu1 N11 C51 -33.82(13) . .
O4 Cu1 N11 C11 145.87(13) . .
N11 Cu1 O1 C1 174.45(12) . .
N11 Cu1 O2 C3 -175.89(12) . .
N11 Cu1 O3 C1 -175.10(14) . 2_666
N11 Cu1 O4 C3 175.21(13) . 2_666
N11 C51 C41 C31 -0.4(3) . .
N21 N31 C61 N21 0.0(3) 2_877 .
N21 N31 C61 C31 179.76(14) 2_877 .
N31 N21 C61 N31 0.0(3) 2_877 .
N31 N21 C61 C31 -179.76(14) 2_877 .
C51 N11 C11 C21 0.7(3) . .
C51 C41 C31 C21 0.7(3) . .
C51 C41 C31 C61 -179.57(16) . .
C41 C31 C21 C11 -0.3(3) . .
C41 C31 C61 N21 -19.9(2) . .
C41 C31 C61 N31 160.29(16) . .
C31 C21 C11 N11 -0.4(3) . .
C21 C31 C61 N21 159.84(16) . .
C21 C31 C61 N31 -20.0(2) . .
C11 N11 C51 C41 -0.3(3) . .
C61 C31 C21 C11 179.91(16) . .
