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#$Date: 2021-12-20 12:09:45 +0200 (Mon, 20 Dec 2021) $
#$Revision: 271523 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/57/1565797.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_1565797
loop_
_publ_author_name
'Azmi, Nurul I.'
'Zhan, Shun-Ze'
'Li, Jing-Hong'
'Razali, Mohd. R.'
_publ_section_title
;
 Metal complexes based on substituted aliphatic acid derived from a
 Diels-Alder adduct: Synthesis and potential ratiometric luminescent
 temperature sensor of d10 complex
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119167
_journal_paper_doi               10.1016/j.ica.2019.119167
_journal_volume                  498
_journal_year                    2019
_chemical_formula_sum            'C42 H39 Cu N2 O11'
_chemical_formula_weight         811.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1083(5)
_cell_length_b                   39.2626(19)
_cell_length_c                   8.5567(5)
_cell_measurement_reflns_used    18374
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      1.50
_cell_volume                     3731.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    X-SEED
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8 Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11630
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.385
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.6273
_exptl_absorpt_correction_T_min  0.4261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1543 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4141
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0417
_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)+(0.0538P)²+2.0392P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                3818
_reflns_number_total             4141
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           a
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_sg_symbol_H-M      'A b a 2'
_cod_database_code               1565797
_shelx_shelxl_version_number     2014/7
_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   0.830
_shelx_estimated_absorpt_t_max   0.880
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z+1/2'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
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 1.0000 0.5000 0.53176(11) 0.04159(19) Uani 1 2 d DS T P . .
O1W O 1.1032(5) 0.54137(12) 0.4574(8) 0.0590(15) Uani 0.6 1 d . . P A 1
O1A O 1.0607(7) 0.52505(19) 0.3461(10) 0.0513(17) Uani 0.4 1 d . U P A 2
O2W O 1.0000 0.5000 0.7654(7) 0.0673(15) Uani 1 2 d S TU P A .
O1 O 0.8581(2) 0.52792(6) 0.5384(5) 0.0532(7) Uani 1 1 d . . . . .
O2 O 0.7155(4) 0.49962(8) 0.4139(5) 0.0620(9) Uani 1 1 d . U . . .
O3 O 0.7753(2) 0.64415(8) 0.4739(4) 0.0521(7) Uani 1 1 d . . . . .
O4 O 0.5101(3) 0.59292(8) 0.8016(4) 0.0513(8) Uani 1 1 d . . . . .
N1 N 0.6572(3) 0.61184(7) 0.6350(4) 0.0377(7) Uani 1 1 d . . . . .
C7 C 0.7526(3) 0.52433(8) 0.4906(4) 0.0365(7) Uani 1 1 d . . . . .
C9 C 0.6651(3) 0.55258(9) 0.5313(5) 0.0386(7) Uani 1 1 d . . . . .
H9A H 0.6314 0.5623 0.4340 0.046 Uiso 1 1 calc R U . . .
H9B H 0.5977 0.5431 0.5932 0.046 Uiso 1 1 calc R U . . .
C10 C 0.7262(4) 0.58022(10) 0.6235(6) 0.0511(11) Uani 1 1 d . . . . .
H10A H 0.7422 0.5717 0.7303 0.061 Uiso 1 1 calc R U . . .
H10B H 0.8048 0.5853 0.5743 0.061 Uiso 1 1 calc R U . . .
C13 C 0.6908(3) 0.64158(9) 0.5611(4) 0.0349(7) Uani 1 1 d . . . . .
C14 C 0.5557(3) 0.61565(9) 0.7278(5) 0.0366(7) Uani 1 1 d . . . . .
C16 C 0.5135(3) 0.65206(10) 0.7176(4) 0.0319(8) Uani 1 1 d . . . . .
H16 H 0.5150 0.6629 0.8234 0.038 Uiso 1 1 calc R U . . .
C17 C 0.6047(3) 0.66940(9) 0.6094(4) 0.0335(7) Uani 1 1 d . . . . .
H17 H 0.6487 0.6878 0.6667 0.040 Uiso 1 1 calc R U . . .
C18 C 0.5406(3) 0.68432(9) 0.4630(4) 0.0351(7) Uani 1 1 d . . . . .
C19 C 0.3855(3) 0.65473(8) 0.6451(4) 0.0315(7) Uani 1 1 d . . . . .
C20 C 0.3630(3) 0.69258(9) 0.6240(4) 0.0361(7) Uani 1 1 d . . . . .
C21 C 0.2728(4) 0.71114(10) 0.6930(5) 0.0471(9) Uani 1 1 d . . . . .
H21 H 0.2158 0.7003 0.7591 0.057 Uiso 1 1 calc R U . . .
C22 C 0.2657(5) 0.74615(10) 0.6650(6) 0.0599(13) Uani 1 1 d . . . . .
H22 H 0.2035 0.7592 0.7121 0.072 Uiso 1 1 calc R U . . .
C23 C 0.3487(5) 0.76167(11) 0.5694(6) 0.0588(12) Uani 1 1 d . . . . .
H23 H 0.3429 0.7854 0.5501 0.071 Uiso 1 1 calc R U . . .
C24 C 0.4402(4) 0.74329(10) 0.5011(5) 0.0472(10) Uani 1 1 d . . . . .
H24 H 0.4982 0.7543 0.4369 0.057 Uiso 1 1 calc R U . . .
C25 C 0.4465(3) 0.70848(8) 0.5274(5) 0.0355(7) Uani 1 1 d . . . . .
C26 C 0.3951(3) 0.63826(9) 0.4866(4) 0.0323(7) Uani 1 1 d . . . . .
C27 C 0.4774(3) 0.65446(10) 0.3877(4) 0.0331(8) Uani 1 1 d . . . . .
C28 C 0.5023(3) 0.64084(13) 0.2409(5) 0.0449(10) Uani 1 1 d . . . . .
H28 H 0.5570 0.6520 0.1726 0.054 Uiso 1 1 calc R U . . .
C29 C 0.4471(4) 0.61117(13) 0.1962(5) 0.0564(12) Uani 1 1 d . . . . .
H29 H 0.4631 0.6019 0.0957 0.068 Uiso 1 1 calc R U . . .
C30 C 0.3679(4) 0.59447(12) 0.2959(6) 0.0545(11) Uani 1 1 d . . . . .
H30 H 0.3327 0.5735 0.2647 0.065 Uiso 1 1 calc R U . . .
C31 C 0.3401(4) 0.60825(10) 0.4410(5) 0.0436(9) Uani 1 1 d . . . . .
H31 H 0.2841 0.5972 0.5079 0.052 Uiso 1 1 calc R U . . .
H1W H 1.0082 0.5190 0.2536 0.22(7) Uiso 1 1 d DR . . B 2
H2 H 0.3236 0.6438 0.7107 0.021(8) Uiso 1 1 d R . . . .
H3 H 0.5951 0.6950 0.3966 0.037(11) Uiso 1 1 d R . . . .
H3W H 1.0522 0.5156 0.8071 0.056 Uiso 0.5 1 d R U P . .
H4W H 1.1675 0.5355 0.4196 0.22(6) Uiso 1 1 d R . . C 1
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'
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'
O O 0.0106 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
O1 Cu1 O1 176.6(2) . 2_765
O1 Cu1 O1A 91.6(2) . 2_765
O1 Cu1 O1A 91.1(2) 2_765 2_765
O1 Cu1 O1A 91.1(2) . .
O1 Cu1 O1A 91.6(2) 2_765 .
O1A Cu1 O1A 73.8(5) 2_765 .
O1 Cu1 O2W 88.30(12) . .
O1 Cu1 O2W 88.30(12) 2_765 .
O1A Cu1 O2W 143.1(2) 2_765 .
O1A Cu1 O2W 143.1(2) . .
O1 Cu1 O1W 90.89(16) . .
O1 Cu1 O1W 90.15(15) 2_765 .
O2W Cu1 O1W 107.75(19) . .
O1 Cu1 O1W 90.15(15) . 2_765
O1 Cu1 O1W 90.89(16) 2_765 2_765
O2W Cu1 O1W 107.75(19) . 2_765
O1W Cu1 O1W 144.5(4) . 2_765
Cu1 O1W H4W 112.4 . .
Cu1 O1A H1W 108.2 . .
Cu1 O2W H3W 112.9 . .
C7 O1 Cu1 134.1(2) . .
C13 N1 C14 113.0(3) . .
C13 N1 C10 123.1(3) . .
C14 N1 C10 123.8(3) . .
O2 C7 O1 124.9(3) . .
O2 C7 C9 118.7(3) . .
O1 C7 C9 116.4(3) . .
C10 C9 C7 111.0(3) . .
C10 C9 H9A 109.4 . .
C7 C9 H9A 109.4 . .
C10 C9 H9B 109.4 . .
C7 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
N1 C10 C9 114.3(3) . .
N1 C10 H10A 108.7 . .
C9 C10 H10A 108.7 . .
N1 C10 H10B 108.7 . .
C9 C10 H10B 108.7 . .
H10A C10 H10B 107.6 . .
O3 C13 N1 124.5(3) . .
O3 C13 C17 127.1(3) . .
N1 C13 C17 108.4(3) . .
O4 C14 N1 124.2(3) . .
O4 C14 C16 127.0(4) . .
N1 C14 C16 108.8(3) . .
C14 C16 C17 104.5(3) . .
C14 C16 C19 111.8(3) . .
C17 C16 C19 109.5(3) . .
C14 C16 H16 110.3 . .
C17 C16 H16 110.3 . .
C19 C16 H16 110.3 . .
C13 C17 C16 105.2(3) . .
C13 C17 C18 110.0(3) . .
C16 C17 C18 110.6(3) . .
C13 C17 H17 110.3 . .
C16 C17 H17 110.3 . .
C18 C17 H17 110.3 . .
C27 C18 C25 108.7(3) . .
C27 C18 C17 105.3(3) . .
C25 C18 C17 105.0(3) . .
C27 C18 H3 113.1 . .
C25 C18 H3 112.9 . .
C17 C18 H3 111.3 . .
C26 C19 C20 109.0(3) . .
C26 C19 C16 105.4(3) . .
C20 C19 C16 105.3(3) . .
C26 C19 H2 112.0 . .
C20 C19 H2 112.3 . .
C16 C19 H2 112.4 . .
C21 C20 C25 120.3(3) . .
C21 C20 C19 126.1(3) . .
C25 C20 C19 113.6(3) . .
C20 C21 C22 119.3(4) . .
C20 C21 H21 120.3 . .
C22 C21 H21 120.3 . .
C23 C22 C21 120.0(4) . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C22 C23 C24 121.0(4) . .
C22 C23 H23 119.5 . .
C24 C23 H23 119.5 . .
C23 C24 C25 119.0(4) . .
C23 C24 H24 120.5 . .
C25 C24 H24 120.5 . .
C24 C25 C20 120.4(3) . .
C24 C25 C18 126.3(3) . .
C20 C25 C18 113.3(3) . .
C31 C26 C27 120.3(3) . .
C31 C26 C19 126.1(3) . .
C27 C26 C19 113.3(3) . .
C28 C27 C26 120.1(4) . .
C28 C27 C18 126.2(4) . .
C26 C27 C18 113.5(3) . .
C29 C28 C27 119.3(4) . .
C29 C28 H28 120.4 . .
C27 C28 H28 120.4 . .
C28 C29 C30 120.8(4) . .
C28 C29 H29 119.6 . .
C30 C29 H29 119.6 . .
C31 C30 C29 120.4(4) . .
C31 C30 H30 119.8 . .
C29 C30 H30 119.8 . .
C26 C31 C30 119.1(4) . .
C26 C31 H31 120.5 . .
C30 C31 H31 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.921(2) .
Cu1 O1 1.921(2) 2_765
Cu1 O1A 1.986(8) 2_765
Cu1 O1A 1.986(8) .
Cu1 O2W 1.999(6) .
Cu1 O1W 2.088(5) .
Cu1 O1W 2.088(5) 2_765
O1W H4W 0.8166 .
O1A H1W 1.0120 .
O2W H3W 0.9172 .
O1 C7 1.249(5) .
O2 C7 1.242(5) .
O3 C13 1.203(5) .
O4 C14 1.205(5) .
N1 C13 1.380(5) .
N1 C14 1.386(5) .
N1 C10 1.462(4) .
C7 C9 1.516(4) .
C9 C10 1.503(5) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C13 C17 1.509(5) .
C14 C16 1.507(5) .
C16 C17 1.532(5) .
C16 C19 1.555(5) .
C16 H16 1.0000 .
C17 C18 1.555(5) .
C17 H17 1.0000 .
C18 C27 1.511(6) .
C18 C25 1.516(5) .
C18 H3 0.9300 .
C19 C26 1.506(5) .
C19 C20 1.518(5) .
C19 H2 0.9860 .
C20 C21 1.372(5) .
C20 C25 1.390(5) .
C21 C22 1.397(6) .
C21 H21 0.9500 .
C22 C23 1.376(7) .
C22 H22 0.9500 .
C23 C24 1.376(6) .
C23 H23 0.9500 .
C24 C25 1.387(5) .
C24 H24 0.9500 .
C26 C31 1.384(5) .
C26 C27 1.399(5) .
C27 C28 1.393(6) .
C28 C29 1.371(7) .
C28 H28 0.9500 .
C29 C30 1.390(7) .
C29 H29 0.9500 .
C30 C31 1.389(6) .
C30 H30 0.9500 .
C31 H31 0.9500 .
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
O1W H4W O2 0.82 1.90 2.604(6) 144.5 2_765
O2W H3W O2 0.92 2.12 2.711(5) 121.3 4_565
