#------------------------------------------------------------------------------
#$Date: 2024-04-05 01:05:43 +0200 (Fri 05 de Apr de 2024) $
#$Revision: 290882 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/80/7248084.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_7248084
loop_
_publ_author_name
'Shore, Madeline C.'
'Nicholas, Aaron D.'
'Vasiliu, Monica'
'Edwards, Kyle C.'
'de Melo, Gabriel F.'
'Bertke, Jeffery A.'
'Dixon, David A.'
'Knope, Karah E.'
_publ_section_title
;
 Structural chemistry of penta- and hexanitrato thorium(iv) complexes
 isolated using N--H donors
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1380
_journal_page_last               1398
_journal_paper_doi               10.1039/D3CE01319G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_sum            'C20 H24 N12 O24 Th'
_chemical_formula_weight         1048.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-06 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.951(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1866(7)
_cell_length_b                   13.3824(9)
_cell_length_c                   13.0890(9)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.08
_cell_volume                     1774.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            57273
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.369
_diffrn_reflns_theta_min         2.521
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.312
_exptl_absorpt_correction_T_max  0.14335
_exptl_absorpt_correction_T_min  0.02160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.704
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0279P)²+1.0068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2931
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01319g2.cif
_cod_data_source_block           mono_a
_cod_depositor_comments
'Adding full bibliography for 7248080--7248089.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7248084
_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.
;
_shelx_estimated_absorpt_t_min   0.365
_shelx_estimated_absorpt_t_max   0.596
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.500000 0.500000 0.500000 0.02510(6) Uani 1 2 d S . P . .
N11 N 0.4928(6) 0.6377(5) 0.3198(5) 0.0355(14) Uani 0.744(3) 1 d D U P A 1
O11 O 0.4110(2) 0.56403(17) 0.32273(16) 0.0333(6) Uani 0.744(3) 1 d D U P A 1
O12 O 0.5803(3) 0.64353(18) 0.39459(19) 0.0338(6) Uani 0.744(3) 1 d D U P A 1
O13 O 0.4857(7) 0.6938(5) 0.2470(5) 0.0663(19) Uani 0.744(3) 1 d D U P A 1
N11B N 0.470(2) 0.6333(17) 0.3146(13) 0.031(2) Uani 0.256(3) 1 d D U P A 2
O11B O 0.4241(7) 0.6563(5) 0.4002(5) 0.0308(15) Uani 0.256(3) 1 d D U P A 2
O12B O 0.5452(7) 0.5578(5) 0.3189(5) 0.0324(15) Uani 0.256(3) 1 d D U P A 2
O13B O 0.4556(13) 0.6958(13) 0.2466(12) 0.024(3) Uani 0.256(3) 1 d D U P A 2
N21 N 0.3140(5) 0.6390(9) 0.5926(7) 0.0295(15) Uani 0.747(3) 1 d D U P B 1
O21 O 0.3624(2) 0.66027(16) 0.50944(17) 0.0301(6) Uani 0.747(3) 1 d D U P B 1
O22 O 0.3658(2) 0.56345(16) 0.64197(17) 0.0318(6) Uani 0.747(3) 1 d D U P B 1
O23 O 0.2241(6) 0.6871(7) 0.6221(5) 0.0354(13) Uani 0.747(3) 1 d D U P B 1
N21B N 0.3205(13) 0.634(3) 0.605(2) 0.030(2) Uani 0.253(3) 1 d D U P A 2
O21B O 0.2773(6) 0.5626(5) 0.5469(5) 0.0322(15) Uani 0.253(3) 1 d D U P A 2
O22B O 0.4465(7) 0.6454(5) 0.6161(5) 0.0326(16) Uani 0.253(3) 1 d D U P A 2
O23B O 0.2467(17) 0.6857(19) 0.6499(14) 0.034(3) Uani 0.253(3) 1 d D U P A 2
N31 N 0.2579(7) 0.3946(5) 0.4007(6) 0.0292(14) Uani 0.749(3) 1 d D U P C 1
O31 O 0.2510(2) 0.4705(2) 0.46341(19) 0.0338(6) Uani 0.749(3) 1 d D U P C 1
O32 O 0.3715(2) 0.36881(17) 0.38545(17) 0.0301(6) Uani 0.749(3) 1 d D U P C 1
O33 O 0.1595(9) 0.3527(9) 0.3617(10) 0.037(2) Uani 0.749(3) 1 d D U P C 1
N31B N 0.253(2) 0.3966(17) 0.414(2) 0.029(2) Uani 0.251(3) 1 d D U P A 2
O31B O 0.3111(6) 0.4620(5) 0.3589(5) 0.0298(15) Uani 0.251(3) 1 d D U P A 2
O32B O 0.3192(7) 0.3676(5) 0.4938(5) 0.0316(16) Uani 0.251(3) 1 d D U P A 2
O33B O 0.152(3) 0.355(2) 0.380(3) 0.030(4) Uani 0.251(3) 1 d D U P A 2
N41 N 0.21084(17) 0.89797(14) 0.47354(14) 0.0232(4) Uani 1 1 d . . . . .
O41 O 0.08904(15) 0.89777(13) 0.47428(13) 0.0330(4) Uani 1 1 d . . . . .
O42 O 0.26088(15) 0.89500(12) 0.38946(11) 0.0284(4) Uani 1 1 d . . . . .
O43 O 0.28466(15) 0.90214(12) 0.55609(11) 0.0277(3) Uani 1 1 d . . . . .
N51 N 0.88168(19) 0.38003(15) 0.78329(15) 0.0275(4) Uani 1 1 d . . . . .
H51A H 0.831(3) 0.372(2) 0.831(2) 0.041 Uiso 1 1 d . U . . .
C51 C 0.9733(2) 0.45162(18) 0.79610(18) 0.0293(5) Uani 1 1 d . . . . .
H51 H 0.980604 0.491392 0.856547 0.035 Uiso 1 1 calc R U . . .
C52 C 1.0567(3) 0.4677(2) 0.7223(2) 0.0342(6) Uani 1 1 d . . . . .
H52 H 1.122102 0.518494 0.730847 0.041 Uiso 1 1 calc R U . . .
C53 C 1.0441(3) 0.4090(2) 0.6356(2) 0.0406(6) Uani 1 1 d . . . . .
H53 H 1.101049 0.418973 0.583375 0.049 Uiso 1 1 calc R U . . .
C54 C 0.9484(3) 0.3354(2) 0.6245(2) 0.0388(6) Uani 1 1 d . . . . .
H54 H 0.938951 0.294865 0.564626 0.047 Uiso 1 1 calc R U . . .
C55 C 0.8677(2) 0.32138(19) 0.70024(19) 0.0328(6) Uani 1 1 d . . . . .
H55 H 0.802260 0.270520 0.693965 0.039 Uiso 1 1 calc R U . . .
N61 N 0.52992(19) 0.87782(14) 0.43488(14) 0.0247(4) Uani 1 1 d . . . . .
H61A H 0.449(3) 0.884(2) 0.419(2) 0.037 Uiso 1 1 d . U . . .
C61 C 0.5764(2) 0.86574(17) 0.53327(17) 0.0271(5) Uani 1 1 d . . . . .
H61 H 0.518227 0.866795 0.585450 0.033 Uiso 1 1 calc R U . . .
C62 C 0.7091(2) 0.85181(19) 0.5580(2) 0.0344(6) Uani 1 1 d . . . . .
H62 H 0.743974 0.844122 0.627780 0.041 Uiso 1 1 calc R U . . .
C63 C 0.7916(2) 0.84903(19) 0.4812(2) 0.0379(6) Uani 1 1 d . . . . .
H63 H 0.883682 0.839182 0.497638 0.045 Uiso 1 1 calc R U . . .
C64 C 0.7400(3) 0.86060(19) 0.3803(2) 0.0383(6) Uani 1 1 d . . . . .
H64 H 0.795813 0.857699 0.326518 0.046 Uiso 1 1 calc R U . . .
C65 C 0.6067(2) 0.87638(17) 0.35846(18) 0.0312(5) Uani 1 1 d . . . . .
H65 H 0.569712 0.886178 0.289549 0.037 Uiso 1 1 calc R U . . .
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'
Th Th -7.2400 8.8979 '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
_geom_angle_publ_flag
O12 Th1 O12 180.0 . 3_666 ?
O12 Th1 O11 50.07(8) . . ?
O12 Th1 O11 129.93(8) 3_666 . ?
O12 Th1 O11 129.93(8) . 3_666 ?
O12 Th1 O11 50.07(8) 3_666 3_666 ?
O11 Th1 O11 180.0 . 3_666 ?
O11B Th1 O32B 68.0(2) . 3_666 ?
O11B Th1 O32B 112.0(2) 3_666 3_666 ?
O12 Th1 O32B 38.95(16) . 3_666 ?
O12 Th1 O32B 141.05(16) 3_666 3_666 ?
O11 Th1 O32B 89.01(16) . 3_666 ?
O11 Th1 O32B 90.99(16) 3_666 3_666 ?
O11B Th1 O32B 112.0(2) . . ?
O11B Th1 O32B 68.0(2) 3_666 . ?
O32B Th1 O32B 180.0 3_666 . ?
O11B Th1 O21B 67.9(2) . . ?
O11B Th1 O21B 112.1(2) 3_666 . ?
O32B Th1 O21B 114.9(2) 3_666 . ?
O32B Th1 O21B 65.1(2) . . ?
O12 Th1 O21B 76.92(16) . 3_666 ?
O12 Th1 O21B 103.08(16) 3_666 3_666 ?
O11 Th1 O21B 97.62(16) . 3_666 ?
O11 Th1 O21B 82.38(16) 3_666 3_666 ?
O11B Th1 O22B 66.9(2) . . ?
O11B Th1 O22B 113.1(2) 3_666 . ?
O32B Th1 O22B 69.6(2) 3_666 . ?
O32B Th1 O22B 110.4(2) . . ?
O21B Th1 O22B 50.1(2) . . ?
O21B Th1 O22B 129.9(2) 3_666 . ?
O12 Th1 O22B 98.70(19) . 3_666 ?
O12 Th1 O22B 81.30(19) 3_666 3_666 ?
O11 Th1 O22B 78.06(18) . 3_666 ?
O11 Th1 O22B 101.94(18) 3_666 3_666 ?
O13 N11 O12 123.8(7) . . ?
O13 N11 O11 120.7(7) . . ?
O12 N11 O11 115.5(3) . . ?
O13 N11 Th1 177.9(5) . . ?
O12 N11 Th1 57.71(19) . . ?
O11 N11 Th1 57.98(18) . . ?
N11 O11 Th1 96.5(3) . . ?
N11 O12 Th1 97.7(3) . . ?
O13B N11B O12B 127.6(11) . . ?
O13B N11B O11B 116.0(14) . . ?
O12B N11B O11B 115.0(8) . . ?
O13B N11B Th1 172.8(17) . . ?
O12B N11B Th1 58.6(5) . . ?
O11B N11B Th1 57.1(5) . . ?
N11B O11B Th1 97.5(6) . . ?
N11B O12B Th1 96.7(6) . . ?
O23 N21 O21 121.6(10) . . ?
O23 N21 O22 122.8(11) . . ?
O21 N21 O22 115.5(3) . . ?
O23 N21 Th1 170.3(5) . . ?
O21 N21 Th1 58.4(2) . . ?
O22 N21 Th1 58.05(18) . . ?
N21 O21 Th1 96.7(4) . . ?
N21 O22 Th1 96.8(4) . . ?
O23B N21B O21B 121.6(17) . . ?
O23B N21B O22B 122.6(16) . . ?
O21B N21B O22B 115.8(9) . . ?
O23B N21B Th1 178(3) . . ?
O21B N21B Th1 57.7(5) . . ?
O22B N21B Th1 58.2(5) . . ?
N21B O21B Th1 97.4(6) . . ?
N21B O22B Th1 96.6(7) . . ?
O33 N31 O32 123.1(11) . . ?
O33 N31 O31 121.7(11) . . ?
O32 N31 O31 115.3(4) . . ?
O33 N31 Th1 179.1(11) . . ?
O32 N31 Th1 57.7(2) . . ?
O31 N31 Th1 57.53(18) . . ?
N31 O31 Th1 96.9(3) . . ?
N31 O32 Th1 98.2(4) . . ?
O33B N31B O32B 122.1(15) . . ?
O33B N31B O31B 120.8(18) . . ?
O32B N31B O31B 115.9(9) . . ?
O33B N31B Th1 179(4) . . ?
O32B N31B Th1 57.9(5) . . ?
O31B N31B Th1 59.4(5) . . ?
N31B O31B Th1 94.7(7) . . ?
N31B O32B Th1 97.7(6) . . ?
O41 N41 O43 120.30(18) . . ?
O41 N41 O42 120.10(18) . . ?
O43 N41 O42 119.59(17) . . ?
C51 N51 C55 122.5(2) . . ?
C51 N51 H51A 117.7(19) . . ?
C55 N51 H51A 119.8(19) . . ?
N51 C51 C52 120.1(2) . . ?
N51 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C51 C52 C53 118.8(2) . . ?
C51 C52 H52 120.6 . . ?
C53 C52 H52 120.6 . . ?
C52 C53 C54 119.8(2) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C55 C54 C53 119.6(2) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
N51 C55 C54 119.2(2) . . ?
N51 C55 H55 120.4 . . ?
C54 C55 H55 120.4 . . ?
C65 N61 C61 123.0(2) . . ?
C65 N61 H61A 116.8(19) . . ?
C61 N61 H61A 120.1(19) . . ?
N61 C61 C62 119.2(2) . . ?
N61 C61 H61 120.4 . . ?
C62 C61 H61 120.4 . . ?
C61 C62 C63 119.5(2) . . ?
C61 C62 H62 120.2 . . ?
C63 C62 H62 120.2 . . ?
C62 C63 C64 119.8(2) . . ?
C62 C63 H63 120.1 . . ?
C64 C63 H63 120.1 . . ?
C65 C64 C63 119.1(2) . . ?
C65 C64 H64 120.5 . . ?
C63 C64 H64 120.5 . . ?
N61 C65 C64 119.4(2) . . ?
N61 C65 H65 120.3 . . ?
C64 C65 H65 120.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O11B 2.544(7) . ?
Th1 O11B 2.544(7) 3_666 ?
Th1 O12 2.549(2) . ?
Th1 O12 2.549(2) 3_666 ?
Th1 O11 2.550(2) . ?
Th1 O11 2.550(2) 3_666 ?
Th1 O32B 2.551(7) 3_666 ?
Th1 O32B 2.551(7) . ?
Th1 O21B 2.552(6) . ?
Th1 O21B 2.552(6) 3_666 ?
Th1 O22B 2.562(7) . ?
Th1 O22B 2.562(7) 3_666 ?
N11 O13 1.209(4) . ?
N11 O12 1.256(8) . ?
N11 O11 1.295(9) . ?
N11B O13B 1.218(8) . ?
N11B O12B 1.263(11) . ?
N11B O11B 1.297(13) . ?
N21 O23 1.215(4) . ?
N21 O21 1.273(13) . ?
N21 O22 1.283(13) . ?
N21B O23B 1.216(8) . ?
N21B O21B 1.272(16) . ?
N21B O22B 1.285(15) . ?
N31 O33 1.214(4) . ?
N31 O32 1.243(10) . ?
N31 O31 1.312(11) . ?
N31B O33B 1.215(8) . ?
N31B O32B 1.244(11) . ?
N31B O31B 1.311(15) . ?
N41 O41 1.242(2) . ?
N41 O43 1.252(2) . ?
N41 O42 1.260(2) . ?
N51 C51 1.336(3) . ?
N51 C55 1.336(3) . ?
N51 H51A 0.86(3) . ?
C51 C52 1.367(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.376(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.383(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.365(4) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
N61 C65 1.332(3) . ?
N61 C61 1.335(3) . ?
N61 H61A 0.84(3) . ?
C61 C62 1.369(3) . ?
C61 H61 0.9500 . ?
C62 C63 1.376(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.379(4) . ?
C63 H63 0.9500 . ?
C64 C65 1.374(4) . ?
C64 H64 0.9500 . ?
C65 H65 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
_geom_hbond_publ_flag
N51 H51A O23^a 0.86(3) 2.62(3) 3.105(6) 117(2) 2_646 yes
N51 H51A O23B^b 0.86(3) 2.63(3) 3.078(16) 114(2) 2_646 yes
N51 H51A N41 0.86(3) 2.66(3) 3.420(3) 149(2) 2_646 yes
N51 H51A O41 0.86(3) 2.61(3) 3.165(3) 123(2) 2_646 yes
N51 H51A O43 0.86(3) 2.02(3) 2.849(2) 161(3) 2_646 yes
N61 H61A N41 0.84(3) 2.61(3) 3.352(3) 149(2) . yes
N61 H61A O42 0.84(3) 1.92(3) 2.753(2) 176(3) . yes
N61 H61A O43 0.84(3) 2.59(3) 3.112(2) 122(2) . yes
