#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:32:23 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228875 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/09/7230983.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_7230983
loop_
_publ_author_name
'Kyratzis, Nicholas'
'Cao, Winnie'
'Izgorodina, Ekaterina I.'
'Turner, David R.'
_publ_section_title
;
 Structural changes in coordination polymers in response to small changes
 in steric bulk (H vs. Me): an experimental and theoretical study
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4115
_journal_paper_doi               10.1039/C8CE00744F
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C30 H18 Cu N4 O8'
_chemical_formula_sum            'C30 H18 Cu N4 O8'
_chemical_formula_weight         626.02
_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
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                115.19(3)
_cell_angle_beta                 105.01(3)
_cell_angle_gamma                96.15(3)
_cell_formula_units_Z            2
_cell_length_a                   11.713(2)
_cell_length_b                   11.938(2)
_cell_length_c                   12.993(3)
_cell_measurement_reflns_used    58526
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.026
_cell_measurement_theta_min      1.841
_cell_volume                     1538.1(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scnas'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1499
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58512
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.029
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             638
_exptl_crystal_recrystallization_method
'Crystallised at elevated temperature from synthesis'
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.672
_refine_diff_density_min         -1.977
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0775
_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/[σ²(Fo²)+(0.1032P)²+1.7322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6408
_reflns_number_total             9276
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00744f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7230978--7230987.cif.'
_cod_original_cell_volume        1538.0(7)
_cod_database_code               7230983
_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_max   0.985
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C30(H30), C28(H28), C29(H29), C9(H9), C19(H19), C24(H24), C21(H21),
 C12(H12), C25(H25), C22(H22), C27(H27), C7(H7), C10(H10)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Cu1 Cu -0.09065(4) 0.38823(4) 0.01323(3) 0.03497(14) Uani 1 1 d .
O8 O 0.8819(2) 0.4961(2) 0.9315(2) 0.0389(5) Uani 1 1 d .
O2 O -0.0321(2) 0.2978(2) 0.1014(2) 0.0384(5) Uani 1 1 d .
O4 O -0.0279(2) 0.3409(3) 0.3615(2) 0.0502(7) Uani 1 1 d .
O7 O 0.6844(3) 0.4003(3) 0.8608(3) 0.0522(7) Uani 1 1 d .
O3 O 0.1440(3) 0.0628(3) 0.1245(3) 0.0535(7) Uani 1 1 d .
N3 N -0.1162(3) 0.5213(3) 0.1577(3) 0.0420(7) Uani 1 1 d .
N1 N 0.0570(3) 0.1980(3) 0.2471(3) 0.0379(6) Uani 1 1 d .
N4 N -0.0867(3) 1.2406(3) 0.8626(2) 0.0388(6) Uani 1 1 d .
O5 O 0.7139(3) 0.3557(3) 0.5999(3) 0.0601(8) Uani 1 1 d .
O1 O -0.2244(3) 0.1970(3) 0.0536(3) 0.0609(8) Uani 1 1 d .
O6 O 0.5444(3) 0.6477(3) 0.8279(3) 0.0662(9) Uani 1 1 d .
N2 N 0.6297(3) 0.5047(3) 0.7091(3) 0.0467(7) Uani 1 1 d .
C6 C 0.1863(3) 0.3761(3) 0.4446(3) 0.0379(7) Uani 1 1 d .
C3 C 0.1568(3) 0.1526(3) 0.2220(3) 0.0401(7) Uani 1 1 d .
C4 C 0.0656(3) 0.3077(3) 0.3514(3) 0.0388(7) Uani 1 1 d .
C5 C 0.2771(3) 0.2166(3) 0.3215(3) 0.0404(7) Uani 1 1 d .
C8 C 0.2879(3) 0.3257(3) 0.4287(3) 0.0373(7) Uani 1 1 d .
C20 C -0.0224(4) 0.5848(3) 0.2628(3) 0.0446(8) Uani 1 1 d .
H20 H 0.051665 0.558327 0.268823 0.053 Uiso 1 1 calc R
C11 C 0.4015(3) 0.3856(3) 0.5227(3) 0.0390(7) Uani 1 1 d .
C18 C 0.7703(4) 0.4766(3) 0.8696(3) 0.0425(8) Uani 1 1 d .
C30 C 0.0178(4) 1.2047(3) 0.8617(3) 0.0433(8) Uani 1 1 d .
H30 H 0.088392 1.251283 0.931841 0.052 Uiso 1 1 calc R
C13 C 0.5033(3) 0.3340(4) 0.5073(4) 0.0440(8) Uani 1 1 d .
C26 C -0.0745(4) 1.0305(3) 0.6605(3) 0.0464(9) Uani 1 1 d .
C28 C 0.0271(4) 1.1026(3) 0.7628(4) 0.0467(8) Uani 1 1 d .
H28 H 0.103548 1.081992 0.765237 0.056 Uiso 1 1 calc R
C14 C 0.4124(3) 0.4951(4) 0.6307(3) 0.0425(7) Uani 1 1 d .
C1 C -0.1123(3) 0.2163(3) 0.0992(3) 0.0390(7) Uani 1 1 d .
C29 C -0.1867(4) 1.1720(4) 0.7625(3) 0.0472(8) Uani 1 1 d .
H29 H -0.261366 1.196614 0.761542 0.057 Uiso 1 1 calc R
C9 C 0.1994(4) 0.4854(4) 0.5487(3) 0.0435(8) Uani 1 1 d .
H9 H 0.131263 0.520366 0.557407 0.052 Uiso 1 1 calc R
C23 C -0.1367(4) 0.7285(3) 0.3565(3) 0.0478(9) Uani 1 1 d .
C15 C 0.6227(4) 0.3953(4) 0.6058(4) 0.0491(9) Uani 1 1 d .
C19 C -0.2225(4) 0.5580(4) 0.1526(3) 0.0462(8) Uani 1 1 d .
H19 H -0.290523 0.511586 0.080097 0.055 Uiso 1 1 calc R
C24 C -0.1530(4) 0.8396(3) 0.4560(3) 0.0491(9) Uani 1 1 d .
H24 H -0.232031 0.854948 0.446862 0.059 Uiso 1 1 calc R
C21 C -0.2358(4) 0.6597(4) 0.2484(4) 0.0496(9) Uani 1 1 d .
H21 H -0.311432 0.682843 0.241191 0.060 Uiso 1 1 calc R
C12 C 0.3133(4) 0.5454(4) 0.6420(3) 0.0437(8) Uani 1 1 d .
H12 H 0.321717 0.620971 0.713186 0.052 Uiso 1 1 calc R
C25 C -0.0613(5) 0.9195(3) 0.5583(4) 0.0498(9) Uani 1 1 d .
H25 H 0.017531 0.903994 0.565901 0.060 Uiso 1 1 calc R
C2 C -0.0646(3) 0.1347(3) 0.1564(3) 0.0404(7) Uani 1 1 d .
H2A H -0.121649 0.115644 0.194678 0.049 Uiso 1 1 calc R
H2B H -0.062041 0.052491 0.092410 0.049 Uiso 1 1 calc R
C22 C -0.0302(4) 0.6884(3) 0.3635(3) 0.0482(9) Uani 1 1 d .
H22 H 0.037643 0.730963 0.436509 0.058 Uiso 1 1 calc R
C16 C 0.5310(4) 0.5566(4) 0.7307(4) 0.0480(9) Uani 1 1 d .
C27 C -0.1842(4) 1.0668(4) 0.6609(3) 0.0496(9) Uani 1 1 d .
H27 H -0.256276 1.020069 0.592500 0.060 Uiso 1 1 calc R
C7 C 0.3777(4) 0.1697(4) 0.3070(4) 0.0519(9) Uani 1 1 d .
H7 H 0.370642 0.097490 0.233634 0.062 Uiso 1 1 calc R
C17 C 0.7472(4) 0.5611(4) 0.8086(4) 0.0511(10) Uani 1 1 d .
H17A H 0.747214 0.646874 0.869010 0.061 Uiso 1 1 calc R
H17B H 0.813703 0.571213 0.776918 0.061 Uiso 1 1 calc R
C10 C 0.4909(4) 0.2295(4) 0.4017(4) 0.0563(10) Uani 1 1 d .
H10 H 0.559776 0.196391 0.391790 0.068 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cu Cu 0.3410 1.2900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0060 '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
O8 Cu1 O8 79.28(10) 1_454 2_666
O8 Cu1 N3 89.87(11) 1_454 .
O8 Cu1 N4 92.08(11) 1_454 1_544
O2 Cu1 O8 90.07(10) . 2_666
O2 Cu1 O8 169.35(11) . 1_454
O2 Cu1 N3 91.18(11) . .
O2 Cu1 N4 88.24(11) . 1_544
N3 Cu1 O8 93.34(12) . 2_666
N3 Cu1 N4 172.52(13) . 1_544
N4 Cu1 O8 94.12(12) 1_544 2_666
Cu1 O8 Cu1 100.72(10) 1_656 2_666
C18 O8 Cu1 114.5(2) . 1_656
C18 O8 Cu1 144.7(2) . 2_666
C1 O2 Cu1 116.2(2) . .
C20 N3 Cu1 119.3(3) . .
C20 N3 C19 117.8(3) . .
C19 N3 Cu1 122.7(2) . .
C3 N1 C4 124.3(3) . .
C3 N1 C2 119.3(3) . .
C4 N1 C2 116.1(3) . .
C30 N4 Cu1 119.3(2) . 1_566
C30 N4 C29 117.8(3) . .
C29 N4 Cu1 122.9(3) . 1_566
C15 N2 C16 125.4(3) . .
C15 N2 C17 116.7(3) . .
C16 N2 C17 117.6(4) . .
C8 C6 C4 119.2(3) . .
C9 C6 C4 120.3(3) . .
C9 C6 C8 120.4(3) . .
O3 C3 N1 120.9(3) . .
O3 C3 C5 122.6(3) . .
N1 C3 C5 116.5(3) . .
O4 C4 N1 118.5(3) . .
O4 C4 C6 123.2(3) . .
N1 C4 C6 118.3(3) . .
C8 C5 C3 119.9(3) . .
C7 C5 C3 119.7(3) . .
C7 C5 C8 120.4(3) . .
C5 C8 C6 121.2(3) . .
C5 C8 C11 119.8(3) . .
C11 C8 C6 119.0(3) . .
N3 C20 H20 118.9 . .
N3 C20 C22 122.2(4) . .
C22 C20 H20 118.9 . .
C8 C11 C13 119.0(3) . .
C8 C11 C14 119.9(3) . .
C14 C11 C13 121.1(3) . .
O8 C18 C17 115.2(3) . .
O7 C18 O8 124.6(3) . .
O7 C18 C17 120.2(3) . .
N4 C30 H30 118.7 . .
N4 C30 C28 122.7(4) . .
C28 C30 H30 118.7 . .
C11 C13 C15 119.5(4) . .
C10 C13 C11 120.0(4) . .
C10 C13 C15 120.5(4) . .
C28 C26 C25 118.4(4) . .
C28 C26 C27 117.4(3) . .
C27 C26 C25 124.1(4) . .
C30 C28 H28 119.9 . .
C26 C28 C30 120.2(4) . .
C26 C28 H28 119.9 . .
C11 C14 C16 120.0(3) . .
C12 C14 C11 120.0(3) . .
C12 C14 C16 120.0(4) . .
O2 C1 C2 115.9(3) . .
O1 C1 O2 125.5(3) . .
O1 C1 C2 118.5(3) . .
N4 C29 H29 118.8 . .
N4 C29 C27 122.4(4) . .
C27 C29 H29 118.8 . .
C6 C9 H9 119.8 . .
C6 C9 C12 120.3(3) . .
C12 C9 H9 119.8 . .
C21 C23 C24 118.0(4) . .
C22 C23 C24 124.1(4) . .
C22 C23 C21 117.9(3) . .
O5 C15 N2 119.5(4) . .
O5 C15 C13 123.3(4) . .
N2 C15 C13 117.2(3) . .
N3 C19 H19 118.6 . .
N3 C19 C21 122.8(4) . .
C21 C19 H19 118.6 . .
C23 C24 H24 118.5 . .
C25 C24 C23 122.9(4) . .
C25 C24 H24 118.5 . .
C23 C21 H21 120.3 . .
C19 C21 C23 119.4(4) . .
C19 C21 H21 120.3 . .
C14 C12 C9 120.3(3) . .
C14 C12 H12 119.8 . .
C9 C12 H12 119.8 . .
C26 C25 H25 117.8 . .
C24 C25 C26 124.5(4) . .
C24 C25 H25 117.8 . .
N1 C2 C1 112.2(3) . .
N1 C2 H2A 109.2 . .
N1 C2 H2B 109.2 . .
C1 C2 H2A 109.2 . .
C1 C2 H2B 109.2 . .
H2A C2 H2B 107.9 . .
C20 C22 H22 120.1 . .
C23 C22 C20 119.8(4) . .
C23 C22 H22 120.1 . .
O6 C16 N2 120.6(4) . .
O6 C16 C14 122.8(4) . .
N2 C16 C14 116.6(4) . .
C26 C27 H27 120.3 . .
C29 C27 C26 119.4(4) . .
C29 C27 H27 120.3 . .
C5 C7 H7 120.2 . .
C5 C7 C10 119.6(4) . .
C10 C7 H7 120.2 . .
N2 C17 C18 110.9(3) . .
N2 C17 H17A 109.5 . .
N2 C17 H17B 109.5 . .
C18 C17 H17A 109.5 . .
C18 C17 H17B 109.5 . .
H17A C17 H17B 108.0 . .
C13 C10 C7 121.2(4) . .
C13 C10 H10 119.4 . .
C7 C10 H10 119.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O8 2.434(3) 2_666
Cu1 O8 1.992(2) 1_454
Cu1 O2 1.937(2) .
Cu1 N3 1.998(3) .
Cu1 N4 2.016(3) 1_544
O8 C18 1.280(5) .
O2 C1 1.263(5) .
O4 C4 1.222(4) .
O7 C18 1.229(5) .
O3 C3 1.220(4) .
N3 C20 1.345(5) .
N3 C19 1.357(5) .
N1 C3 1.397(4) .
N1 C4 1.397(5) .
N1 C2 1.460(5) .
N4 C30 1.341(5) .
N4 C29 1.354(5) .
O5 C15 1.221(5) .
O1 C1 1.243(4) .
O6 C16 1.222(5) .
N2 C15 1.394(6) .
N2 C16 1.404(5) .
N2 C17 1.469(5) .
C6 C4 1.469(5) .
C6 C8 1.413(5) .
C6 C9 1.379(5) .
C3 C5 1.492(5) .
C5 C8 1.407(5) .
C5 C7 1.380(5) .
C8 C11 1.409(5) .
C20 H20 0.9500 .
C20 C22 1.401(5) .
C11 C13 1.421(5) .
C11 C14 1.415(5) .
C18 C17 1.531(5) .
C30 H30 0.9500 .
C30 C28 1.385(5) .
C13 C15 1.479(5) .
C13 C10 1.364(6) .
C26 C28 1.382(6) .
C26 C25 1.481(5) .
C26 C27 1.400(6) .
C28 H28 0.9500 .
C14 C12 1.376(5) .
C14 C16 1.480(5) .
C1 C2 1.528(4) .
C29 H29 0.9500 .
C29 C27 1.392(5) .
C9 H9 0.9500 .
C9 C12 1.407(5) .
C23 C24 1.479(5) .
C23 C21 1.401(6) .
C23 C22 1.378(6) .
C19 H19 0.9500 .
C19 C21 1.379(5) .
C24 H24 0.9500 .
C24 C25 1.338(6) .
C21 H21 0.9500 .
C12 H12 0.9500 .
C25 H25 0.9500 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C22 H22 0.9500 .
C27 H27 0.9500 .
C7 H7 0.9500 .
C7 C10 1.409(6) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C10 H10 0.9500 .
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 0.500 1.020 0.857 372 94 ' '
