#------------------------------------------------------------------------------
#$Date: 2019-11-08 03:00:49 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/87/7058784.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_7058784
loop_
_publ_author_name
'Kumar, Manesh'
'Qiu, Cheng-Qiang'
'Zaręba, Jan K.'
'Frontera, Antonio'
'Jassal, Amanpreet Kaur'
'Sahoo, Subash Chandra'
'Liu, Sui-Jun'
'Sheikh, Haq Nawaz'
_publ_section_title
;
 Magnetic, luminescence, topological and theoretical studies of
 structurally diverse supramolecular lanthanide coordination polymers with
 flexible glutaric acid as a linker
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14546
_journal_paper_doi               10.1039/C9NJ03664D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '0.25(C60 H88 O56 Tb8), 4(H2 O)'
_chemical_formula_sum            'C15 H30 O18 Tb2'
_chemical_formula_weight         816.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-13
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-08-01 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9368(2)
_cell_length_b                   14.9436(3)
_cell_length_c                   19.6279(4)
_cell_measurement_reflns_used    6843
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3580
_cell_measurement_theta_min      3.2511
_cell_volume                     2320.83(9)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8766
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.434
_diffrn_reflns_theta_min         3.431
_exptl_absorpt_coefficient_mu    6.132
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.370
_refine_diff_density_min         -2.105
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0533P)²+4.1990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2336
_reflns_number_total             2453
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj03664d2.cif
_cod_data_source_block           kasm-c3b
_cod_depositor_comments
'Adding full bibliography for 7058784--7058791.cif.'
_cod_database_code               7058784
_shelx_shelxl_version_number     2018/3
_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,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 O9, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H8A(0.5) H8B(0.5)
4.a Riding coordinates:
 O9(H9A,H9B)
4.b Free rotating group:
 O8(H8C,H8D)
4.c Rotating group:
 O7(H7A,H7B)
4.d Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C2(H2A,H2B), C7(H7C,H7D), C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
Tb1 Tb 0.75642(2) 0.46278(2) 0.51225(2) 0.01394(11) Uani 1 1 d . . .
O3 O 0.8328(4) 0.3228(2) 0.57192(16) 0.0225(7) Uani 1 1 d . . .
O1 O 0.4949(4) 0.45518(18) 0.5612(2) 0.0230(8) Uani 1 1 d . . .
O4 O 0.8531(4) 0.44634(19) 0.63077(19) 0.0247(7) Uani 1 1 d . . .
O2 O 0.2362(4) 0.4533(2) 0.5915(2) 0.0270(8) Uani 1 1 d . . .
O5 O 0.4881(4) 0.07824(18) 0.53318(16) 0.0200(6) Uani 1 1 d . . .
O7 O 0.6159(4) 0.35489(19) 0.44009(18) 0.0259(7) Uani 1 1 d . . .
H7A H 0.668472 0.305062 0.443828 0.039 Uiso 1 1 d GR . .
H7B H 0.614735 0.373181 0.398844 0.039 Uiso 1 1 d GR . .
O6 O 0.2327(4) 0.11377(18) 0.55790(19) 0.0247(7) Uani 1 1 d . . .
C1 C 0.3858(5) 0.4269(2) 0.6006(2) 0.0141(8) Uani 1 1 d . . .
C5 C 0.3858(5) 0.1348(3) 0.5554(2) 0.0164(8) Uani 1 1 d . . .
C6 C 0.8711(5) 0.3628(3) 0.6278(2) 0.0164(8) Uani 1 1 d . . .
C4 C 0.4515(6) 0.2250(3) 0.5777(3) 0.0272(10) Uani 1 1 d . . .
H4A H 0.443022 0.264816 0.538612 0.033 Uiso 1 1 calc R . .
H4B H 0.570225 0.219360 0.592970 0.033 Uiso 1 1 calc R . .
C8 C 1.000000 0.3664(4) 0.750000 0.0244(13) Uani 1 2 d S T P
H8A H 0.911818 0.404603 0.765447 0.029 Uiso 0.5 1 calc R . .
C2 C 0.4312(5) 0.3598(3) 0.6557(2) 0.0193(8) Uani 1 1 d . . .
H2A H 0.385305 0.378569 0.697771 0.023 Uiso 1 1 calc R . .
H2B H 0.553168 0.356322 0.663836 0.023 Uiso 1 1 calc R . .
C7 C 0.9273(5) 0.3096(3) 0.6905(2) 0.0213(9) Uani 1 1 d . . .
H7C H 1.012037 0.266732 0.678822 0.026 Uiso 1 1 calc R . .
H7D H 0.831459 0.276260 0.704970 0.026 Uiso 1 1 calc R . .
C3 C 0.3601(7) 0.2671(3) 0.6344(3) 0.0263(10) Uani 1 1 d . . .
H3A H 0.368935 0.227812 0.673889 0.032 Uiso 1 1 calc R . .
H3B H 0.241227 0.273097 0.619460 0.032 Uiso 1 1 calc R . .
O8 O 0.610(2) 0.0925(4) 0.6998(4) 0.177(5) Uani 1 1 d . U .
H8C H 0.557629 0.045076 0.709785 0.265 Uiso 1 1 d G . .
H8D H 0.715019 0.082021 0.701077 0.265 Uiso 1 1 d G . .
O9 O 0.8810(15) 0.0708(7) 0.7853(7) 0.200(5) Uani 1 1 d . U .
H9A H 0.876319 0.083140 0.827370 0.299 Uiso 1 1 d R . .
H9B H 0.871919 0.014650 0.779490 0.299 Uiso 1 1 d R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Tb Tb -0.1723 4.1537 '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 Tb1 O1 142.91(10) . 5_666
O3 Tb1 O5 110.78(10) . 3
O3 Tb1 C1 155.81(10) . 5_666
O3 Tb1 C5 123.62(11) . 3
O3 Tb1 C6 26.74(11) . .
O1 Tb1 O3 87.54(10) . .
O1 Tb1 O1 66.23(14) . 5_666
O1 Tb1 O4 79.94(13) . .
O1 Tb1 O2 116.89(12) . 5_666
O1 Tb1 O5 162.15(10) . 7_656
O1 Tb1 O5 128.19(10) . 3
O1 Tb1 O7 79.77(12) . .
O1 Tb1 O6 78.42(10) . 3
O1 Tb1 C1 92.06(12) . 5_666
O1 Tb1 C1 25.96(10) 5_666 5_666
O1 Tb1 C5 103.23(11) . 3
O1 Tb1 C5 89.03(10) 5_666 3
O1 Tb1 C6 149.65(11) 5_666 .
O1 Tb1 C6 83.42(12) . .
O4 Tb1 O3 53.27(10) . .
O4 Tb1 O1 137.61(11) . 5_666
O4 Tb1 O5 74.92(10) . 3
O4 Tb1 O6 76.54(11) . 3
O4 Tb1 C1 150.20(10) . 5_666
O4 Tb1 C5 74.11(11) . 3
O4 Tb1 C6 26.53(11) . .
O2 Tb1 O3 146.23(11) 5_666 .
O2 Tb1 O1 50.72(10) 5_666 5_666
O2 Tb1 O4 148.07(11) 5_666 .
O2 Tb1 O5 73.49(11) 5_666 3
O2 Tb1 O6 80.57(11) 5_666 3
O2 Tb1 C1 24.83(11) 5_666 5_666
O2 Tb1 C5 75.56(12) 5_666 3
O2 Tb1 C6 159.58(11) 5_666 .
O5 Tb1 O3 76.76(10) 7_656 .
O5 Tb1 O1 122.95(11) 7_656 5_666
O5 Tb1 O1 106.11(9) 3 5_666
O5 Tb1 O4 96.92(11) 7_656 .
O5 Tb1 O2 74.68(10) 7_656 5_666
O5 Tb1 O5 66.64(11) 7_656 3
O5 Tb1 O7 88.60(11) 7_656 .
O5 Tb1 O6 118.18(10) 7_656 3
O5 Tb1 C1 88.34(10) 3 5_666
O5 Tb1 C1 98.79(11) 7_656 5_666
O5 Tb1 C5 92.64(11) 7_656 3
O5 Tb1 C5 26.29(10) 3 3
O5 Tb1 C6 92.65(11) 3 .
O5 Tb1 C6 86.17(11) 7_656 .
O7 Tb1 O3 77.99(10) . .
O7 Tb1 O1 72.08(10) . 5_666
O7 Tb1 O4 127.53(11) . .
O7 Tb1 O2 83.65(12) . 5_666
O7 Tb1 O5 149.73(11) . 3
O7 Tb1 O6 143.44(10) . 3
O7 Tb1 C1 78.13(11) . 5_666
O7 Tb1 C5 158.03(11) . 3
O7 Tb1 C6 103.22(11) . .
O6 Tb1 O3 129.57(11) 3 .
O6 Tb1 O1 72.39(10) 3 5_666
O6 Tb1 O5 52.13(9) 3 3
O6 Tb1 C1 73.73(11) 3 5_666
O6 Tb1 C5 25.84(10) 3 3
O6 Tb1 C6 103.00(12) 3 .
C5 Tb1 C1 80.00(11) 3 5_666
C6 Tb1 C1 174.93(11) . 5_666
C6 Tb1 C5 98.75(12) . 3
C6 O3 Tb1 92.6(2) . .
Tb1 O1 Tb1 113.77(14) . 5_666
C1 O1 Tb1 88.1(2) . 5_666
C1 O1 Tb1 157.3(3) . .
C6 O4 Tb1 94.9(3) . .
C1 O2 Tb1 101.6(3) . 5_666
Tb1 O5 Tb1 113.36(11) 7_656 3_445
C5 O5 Tb1 153.2(3) . 7_656
C5 O5 Tb1 91.9(2) . 3_445
Tb1 O7 H7A 109.8 . .
Tb1 O7 H7B 108.6 . .
H7A O7 H7B 109.2 . .
C5 O6 Tb1 96.6(2) . 3_445
O1 C1 Tb1 66.0(2) . 5_666
O1 C1 C2 121.5(4) . .
O2 C1 Tb1 53.6(2) . 5_666
O2 C1 O1 119.3(4) . .
O2 C1 C2 119.2(4) . .
C2 C1 Tb1 169.6(3) . 5_666
O5 C5 Tb1 61.8(2) . 3_445
O5 C5 C4 118.8(4) . .
O6 C5 Tb1 57.6(2) . 3_445
O6 C5 O5 119.4(4) . .
O6 C5 C4 121.9(4) . .
C4 C5 Tb1 179.4(3) . 3_445
O3 C6 Tb1 60.7(2) . .
O3 C6 C7 119.8(4) . .
O4 C6 Tb1 58.6(2) . .
O4 C6 O3 119.2(4) . .
O4 C6 C7 120.9(4) . .
C7 C6 Tb1 178.2(3) . .
C5 C4 H4A 108.6 . .
C5 C4 H4B 108.6 . .
C5 C4 C3 114.4(4) . .
H4A C4 H4B 107.6 . .
C3 C4 H4A 108.6 . .
C3 C4 H4B 108.6 . .
C7 C8 H8A 109.2 . .
C7 C8 H8A 109.2 2_756 .
C7 C8 C7 112.2(5) . 2_756
C1 C2 H2A 109.6 . .
C1 C2 H2B 109.6 . .
C1 C2 C3 110.1(4) . .
H2A C2 H2B 108.1 . .
C3 C2 H2A 109.6 . .
C3 C2 H2B 109.6 . .
C6 C7 C8 113.9(3) . .
C6 C7 H7C 108.8 . .
C6 C7 H7D 108.8 . .
C8 C7 H7C 108.8 . .
C8 C7 H7D 108.8 . .
H7C C7 H7D 107.7 . .
C4 C3 C2 112.8(4) . .
C4 C3 H3A 109.0 . .
C4 C3 H3B 109.0 . .
C2 C3 H3A 109.0 . .
C2 C3 H3B 109.0 . .
H3A C3 H3B 107.8 . .
H8C O8 H8D 109.5 . .
H9A O9 H9B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O3 2.450(3) .
Tb1 O1 2.357(3) .
Tb1 O1 2.666(4) 5_666
Tb1 O4 2.405(4) .
Tb1 O2 2.396(4) 5_666
Tb1 O5 2.359(3) 7_656
Tb1 O5 2.531(3) 3
Tb1 O7 2.367(3) .
Tb1 O6 2.440(3) 3
Tb1 C1 2.918(4) 5_666
Tb1 C5 2.871(4) 3
Tb1 C6 2.807(4) .
O3 C6 1.265(5) .
O1 C1 1.278(5) .
O4 C6 1.259(5) .
O2 C1 1.251(5) .
O5 C5 1.273(5) .
O7 H7A 0.8538 .
O7 H7B 0.8539 .
O6 C5 1.260(5) .
C1 C2 1.497(5) .
C5 C4 1.498(6) .
C6 C7 1.503(6) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C3 1.512(7) .
C8 H8A 0.9700 .
C8 C7 1.520(5) 2_756
C8 C7 1.520(5) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 C3 1.541(6) .
C7 H7C 0.9700 .
C7 H7D 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
O8 H8C 0.8498 .
O8 H8D 0.8501 .
O9 H9A 0.8504 .
O9 H9B 0.8496 .
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
_geom_hbond_publ_flag
O7 H7A O3 0.85 1.94 2.700(4) 148.3 7_656 yes
O8 H8D O9 0.85 2.04 2.645(17) 127.7 . yes
