#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:48:21 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229693 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/79/7047952.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_7047952
loop_
_publ_author_name
'Kumar, Gulshan'
'Hussain, Firasat'
'Gupta, Rajeev'
_publ_section_title
;
 Copper based coordination polymers based on metalloligands: utilization
 as heterogeneous oxidation catalysts.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16985
_journal_page_last               16994
_journal_paper_doi               10.1039/c8dt03836h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.25(C84 H52 Co2 Cu2.3 N12 O28), 3.25(O)'
_chemical_formula_sum            'C21 H11 Co0.5 Cu0.58 N3 O10.25'
_chemical_formula_weight         535.41
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-21 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   15.440(5)
_cell_length_b                   15.440(5)
_cell_length_c                   26.265(5)
_cell_measurement_reflns_used    5400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5910
_cell_measurement_theta_min      3.0570
_cell_volume                     6261(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29481
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.050
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             2162
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0936P)²+33.9488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2044
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2558
_reflns_number_total             2954
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03836h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7047952.cif.'
_cod_original_cell_volume        6261(4)
_cod_original_formula_sum        'C21 H11 Co0.50 Cu0.58 N3 O10.25'
_cod_database_code               7047952
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -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
C1 C 0.3888(3) 0.3195(3) 0.41608(15) 0.0309(9) Uani 1 1 d . . .
C2 C 0.4101(3) 0.2724(3) 0.36772(15) 0.0297(9) Uani 1 1 d . . .
C3 C 0.4958(3) 0.2548(3) 0.35579(18) 0.0389(10) Uani 1 1 d . . .
C4 C 0.5168(3) 0.2091(3) 0.31208(18) 0.0399(11) Uani 1 1 d . . .
C5 C 0.4519(3) 0.1789(3) 0.27994(15) 0.0311(9) Uani 1 1 d . . .
C6 C 0.3670(3) 0.1991(4) 0.29126(19) 0.0441(12) Uani 1 1 d . . .
C7 C 0.3463(3) 0.2453(3) 0.33465(19) 0.0436(12) Uani 1 1 d . . .
C8 C 0.4679(3) 0.1477(3) 0.19112(17) 0.0393(11) Uani 1 1 d . . .
C9 C 0.4864(3) 0.0742(3) 0.15513(16) 0.0378(10) Uani 1 1 d . . .
C10 C 0.4870(5) 0.0762(4) 0.1030(2) 0.069(2) Uani 1 1 d . . .
C11 C 0.500000 0.000000 0.0770(3) 0.087(4) Uani 1 2 d S T P
H11 H 0.500000 -0.000001 0.041633 0.105 Uiso 1 2 calc RS T P
Co1 Co 0.500000 0.000000 0.250000 0.0242(3) Uani 1 4 d S T P
Cu1 Cu 0.56676(8) 0.35189(8) 0.500000 0.0303(5) Uani 0.576(4) 2 d S T P
N1 N 0.4735(2) 0.1226(2) 0.23914(13) 0.0310(8) Uani 1 1 d . . .
N2 N 0.500000 0.000000 0.17958(18) 0.0289(10) Uani 1 2 d S T P
O1 O 0.500000 0.500000 0.500000 0.0242(15) Uiso 1 8 d S T P
O2 O 0.4129(6) 0.1881(6) 0.000000 0.108(3) Uani 1 2 d S T P
O3 O 0.3116(2) 0.3298(2) 0.42930(13) 0.0434(8) Uani 1 1 d . . .
O4 O 0.4479(3) 0.2209(2) 0.17474(14) 0.0633(12) Uani 1 1 d . . .
O5 O 0.4502(2) 0.3493(2) 0.44220(12) 0.0403(8) Uani 1 1 d . . .
O7 O 0.3436(3) 0.2580(4) 0.08931(19) 0.0825(14) Uani 1 1 d . . .
O10 O 0.5453(6) 0.1997(5) 0.500000 0.070(2) Uani 1 2 d S T P
H10A H 0.506(5) 0.180(5) 0.500000 0.03(2) Uiso 1 2 d S T P
H3 H 0.547(4) 0.269(4) 0.376(2) 0.054(15) Uiso 1 1 d . . .
H4 H 0.573(3) 0.200(3) 0.3036(17) 0.029(11) Uiso 1 1 d . . .
H6 H 0.328(4) 0.181(4) 0.274(2) 0.066(19) Uiso 1 1 d . . .
H7 H 0.290(4) 0.263(4) 0.343(2) 0.053(16) Uiso 1 1 d . . .
H10 H 0.476(5) 0.114(5) 0.087(3) 0.09(3) Uiso 1 1 d . . .
H10B H 0.586(10) 0.173(10) 0.500000 0.14(7) Uiso 1 2 d S T P
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'
Co Co 0.3494 0.9721 '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'
H H 0.0000 0.0000 '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
O3 C1 C2 120.3(4) . .
O3 C1 O5 121.3(4) . .
O5 C1 C2 118.4(4) . .
C3 C2 C1 119.6(4) . .
C7 C2 C1 121.6(4) . .
C7 C2 C3 118.7(4) . .
C4 C3 C2 120.7(4) . .
C3 C4 C5 120.3(4) . .
C4 C5 N1 119.6(4) . .
C6 C5 C4 118.5(4) . .
C6 C5 N1 121.6(4) . .
C5 C6 C7 120.9(4) . .
C2 C7 C6 120.7(4) . .
N1 C8 C9 111.4(4) . .
O4 C8 C9 120.9(4) . .
O4 C8 N1 127.6(4) . .
C10 C9 C8 127.8(4) . .
N2 C9 C8 112.1(4) . .
N2 C9 C10 120.0(5) . .
C9 C10 C11 118.6(5) . .
C10 C11 C10 120.5(7) . 2_655
N1 Co1 N1 91.22(3) . 16_545
N1 Co1 N1 91.22(3) . 15
N1 Co1 N1 163.2(2) . 2_655
N1 Co1 N1 163.2(2) 15 16_545
N1 Co1 N1 91.22(3) 15 2_655
N1 Co1 N1 91.22(3) 16_545 2_655
N2 Co1 N1 98.38(10) . 15
N2 Co1 N1 81.62(10) . .
N2 Co1 N1 98.38(10) 15 2_655
N2 Co1 N1 81.62(10) 15 15
N2 Co1 N1 98.38(10) . 16_545
N2 Co1 N1 81.62(10) . 2_655
N2 Co1 N1 98.38(10) 15 .
N2 Co1 N1 81.62(10) 15 16_545
N2 Co1 N2 180.0 . 15
O5 Cu1 O5 80.29(16) . 10_556
O5 Cu1 O10 82.90(19) 10_556 .
O5 Cu1 O10 82.90(19) . .
C5 N1 Co1 122.1(3) . .
C8 N1 C5 121.7(4) . .
C8 N1 Co1 115.9(3) . .
C9 N2 C9 122.3(5) 2_655 .
C9 N2 Co1 118.9(3) . .
C9 N2 Co1 118.9(3) 2_655 .
C1 O5 Cu1 159.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.500(6) .
C1 O3 1.253(5) .
C1 O5 1.257(5) .
C2 C3 1.386(6) .
C2 C7 1.378(6) .
C3 C4 1.386(6) .
C4 C5 1.391(6) .
C5 C6 1.380(7) .
C5 N1 1.419(5) .
C6 C7 1.382(7) .
C8 C9 1.505(6) .
C8 N1 1.322(6) .
C8 O4 1.248(6) .
C9 C10 1.369(7) .
C9 N2 1.330(5) .
C10 C11 1.374(7) .
Co1 N1 1.958(4) 15
Co1 N1 1.958(4) 16_545
Co1 N1 1.958(4) .
Co1 N1 1.958(4) 2_655
Co1 N2 1.850(5) .
Co1 N2 1.850(5) 15
Cu1 O5 2.355(3) .
Cu1 O5 2.355(3) 10_556
Cu1 O10 2.373(7) .
