#------------------------------------------------------------------------------
#$Date: 2024-08-05 21:49:26 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293824 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/64/7716443.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_7716443
loop_
_publ_author_name
'Chowdhury, Tajrian'
'Wilson, Claire'
'Farnaby, Joy H.'
_publ_section_title
;
 Activation and functionalisation of carbon dioxide by
 bis-tris(pyrazolyl)borate-supported divalent samarium and trivalent
 lanthanide silylamide complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11884
_journal_page_last               11894
_journal_paper_doi               10.1039/d4dt01382d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C38 H40 B4 N24 O4 Sm2'
_chemical_formula_sum            'C38 H40 B4 N24 O4 Sm2'
_chemical_formula_weight         1240.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-14 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9732(6)
_cell_length_b                   28.6287(8)
_cell_length_c                   21.4608(6)
_cell_measurement_reflns_used    17316
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.0050
_cell_measurement_theta_min      1.4840
_cell_volume                     12885.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ      0.00 180.00   0.20    0.20   0.00   0.00   0.00    --   900
  2  ω   -145.00  25.00   0.20    0.20    --   30.00   0.00   0.00  850
  3  ω   -145.00  25.00   0.20    0.20    --   30.00   0.00 120.00  850
  4  ω   -145.00  25.00   0.20    0.20    --   30.00   0.00 240.00  850
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0323682500
_diffrn_orient_matrix_UB_12      -0.0039042000
_diffrn_orient_matrix_UB_13      -0.0018900500
_diffrn_orient_matrix_UB_21      0.0039588500
_diffrn_orient_matrix_UB_22      -0.0100231000
_diffrn_orient_matrix_UB_23      -0.0289426500
_diffrn_orient_matrix_UB_31      0.0040154500
_diffrn_orient_matrix_UB_32      -0.0215103000
_diffrn_orient_matrix_UB_33      0.0137762500
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54122
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.476
_diffrn_reflns_theta_min         1.486
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.558
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         9847
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0840P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7474
_reflns_number_total             9847
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01382d2.cif
_cod_data_source_block           2_Sm_SmTp2_2_u_C2O4
_cod_depositor_comments
'Adding full bibliography for 7716442--7716448.cif.'
_cod_database_code               7716443
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H40B4N24O4Sm2
_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   0.846
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.72(3)
 0.28(3)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C12(H12)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.780
_oxdiff_exptl_absorpt_empirical_full_min 0.466
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
N11 N 0.5533(3) 0.5345(2) 0.3359(4) 0.0616(16) Uani 1 1 d . . . . .
B1 B 0.3591(5) 0.4473(4) 0.7976(5) 0.060(2) Uani 1 1 d . . . . .
H1 H 0.318739 0.431431 0.818433 0.072 Uiso 1 1 calc R U . . .
B2 B 0.6600(5) 0.4975(3) 0.3637(5) 0.051(2) Uani 1 1 d . . . . .
H2 H 0.706230 0.495918 0.343821 0.061 Uiso 1 1 calc R U . . .
C1 C 0.3458(4) 0.5075(3) 0.6504(4) 0.0539(18) Uani 1 1 d . . . . .
H1A H 0.361884 0.525063 0.616294 0.065 Uiso 1 1 calc R U . . .
N3 N 0.4326(4) 0.5138(3) 0.8230(3) 0.0616(16) Uani 1 1 d . . . . .
C2 C 0.2835(4) 0.4938(3) 0.6556(4) 0.062(2) Uani 1 1 d . . . . .
H2A H 0.249698 0.499485 0.627157 0.075 Uiso 1 1 calc R U . . .
C3 C 0.2809(4) 0.4707(3) 0.7100(4) 0.0585(18) Uani 1 1 d . . . . .
H3 H 0.243705 0.456770 0.727118 0.070 Uiso 1 1 calc R U . . .
C4 C 0.4422(5) 0.5431(4) 0.8743(4) 0.074(2) Uani 1 1 d . . . . .
H4 H 0.473342 0.567132 0.876486 0.089 Uiso 1 1 calc R U . . .
N7 N 0.6103(3) 0.5318(2) 0.4622(3) 0.0509(14) Uani 1 1 d . . . . .
C6 C 0.3666(5) 0.4951(3) 0.8999(4) 0.063(2) Uani 1 1 d . . . . .
H6 H 0.335125 0.478782 0.923115 0.075 Uiso 1 1 calc R U . . .
C7 C 0.4986(3) 0.3797(3) 0.7539(5) 0.058(2) Uani 1 1 d . . . . .
H7 H 0.539915 0.376451 0.736395 0.069 Uiso 1 1 calc R U . . .
C8 C 0.4620(4) 0.3430(3) 0.7776(4) 0.0619(19) Uani 1 1 d . . . . .
H8 H 0.474128 0.311072 0.780478 0.074 Uiso 1 1 calc R U . . .
C9 C 0.4063(5) 0.3617(3) 0.7953(5) 0.072(2) Uani 1 1 d . . . . .
H9 H 0.370336 0.345599 0.811462 0.087 Uiso 1 1 calc R U . . .
C10 C 0.6300(4) 0.5579(3) 0.5076(4) 0.0622(19) Uani 1 1 d . . . . .
H10 H 0.603014 0.569882 0.539361 0.075 Uiso 1 1 calc R U . . .
C5 C 0.4013(6) 0.5326(4) 0.9195(4) 0.082(3) Uani 1 1 d . . . . .
H5 H 0.397078 0.548277 0.958332 0.098 Uiso 1 1 calc R U . . .
C11 C 0.6946(5) 0.5663(3) 0.5045(4) 0.071(2) Uani 1 1 d . . . . .
H11 H 0.720123 0.583734 0.532738 0.086 Uiso 1 1 calc R U . . .
N1 N 0.3818(3) 0.4933(2) 0.6986(4) 0.0513(14) Uani 1 1 d . . . . .
N5 N 0.4676(3) 0.41947(19) 0.7594(3) 0.0492(13) Uani 1 1 d . . . . .
C13 C 0.5739(4) 0.3931(2) 0.4107(3) 0.0518(16) Uani 1 1 d . . . . .
H13 H 0.538923 0.377223 0.429147 0.062 Uiso 1 1 calc R U . . .
N9 N 0.5773(3) 0.4398(2) 0.4002(3) 0.0511(14) Uani 1 1 d . . . . .
C14 C 0.6291(4) 0.3724(3) 0.3904(4) 0.062(2) Uani 1 1 d . . . . .
H14 H 0.639097 0.340040 0.391412 0.075 Uiso 1 1 calc R U . . .
O1 O 0.4875(3) 0.54617(19) 0.6327(3) 0.0498(12) Uani 1 1 d . . . . .
C15 C 0.6663(4) 0.4073(3) 0.3685(3) 0.0532(16) Uani 1 1 d . . . . .
H15 H 0.707634 0.403482 0.351251 0.064 Uiso 1 1 calc R U . . .
C16 C 0.5286(5) 0.5574(4) 0.2897(4) 0.072(2) Uani 1 1 d . . . . .
H16 H 0.485818 0.568324 0.289118 0.086 Uiso 1 1 calc R U . . .
C17 C 0.5696(6) 0.5640(4) 0.2428(5) 0.096(4) Uani 1 1 d . . . . .
H17 H 0.563101 0.580793 0.205203 0.116 Uiso 1 1 calc R U . . .
C18 C 0.6259(5) 0.5397(4) 0.2628(4) 0.077(3) Uani 1 1 d . . . . .
H18 H 0.663922 0.535680 0.239404 0.093 Uiso 1 1 calc R U . . .
C22 C 0.4935(3) 0.5263(2) 0.5809(6) 0.0477(14) Uani 1 1 d . . . . .
Sm1 Sm 0.500000 0.500000 0.72655(2) 0.04429(17) Uani 1 2 d S T P . .
C12 C 0.7134(4) 0.5438(3) 0.4520(4) 0.0534(16) Uani 1 1 d . . . . .
H12 H 0.755866 0.542572 0.436647 0.064 Uiso 1 1 calc R U . . .
N2 N 0.3398(3) 0.4701(2) 0.7366(3) 0.0508(14) Uani 1 1 d . . . . .
N4 N 0.3854(3) 0.4854(3) 0.8413(3) 0.0565(15) Uani 1 1 d . . . . .
N6 N 0.4118(3) 0.40925(19) 0.7852(3) 0.0514(13) Uani 1 1 d . . . . .
N8 N 0.6634(3) 0.5239(2) 0.4254(3) 0.0531(14) Uani 1 1 d . . . . .
N10 N 0.6358(3) 0.4477(2) 0.3751(3) 0.0479(14) Uani 1 1 d . . . . .
N12 N 0.6153(3) 0.5242(2) 0.3193(3) 0.0555(15) Uani 1 1 d . . . . .
O2 O 0.4834(3) 0.54471(19) 0.5292(3) 0.0518(12) Uani 1 1 d . . . . .
Sm2 Sm 0.500000 0.500000 0.43463(2) 0.04434(17) Uani 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 0.0019 0.0015 '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'
B B 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0071 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.5577 3.2693 '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
C16 N11 N12 106.7(7) . . ?
C16 N11 Sm2 130.2(6) . . ?
N12 N11 Sm2 122.4(5) . . ?
N2 B1 H1 109.5 . . ?
N2 B1 N4 108.4(7) . . ?
N2 B1 N6 109.8(7) . . ?
N4 B1 H1 109.5 . . ?
N4 B1 N6 110.0(7) . . ?
N6 B1 H1 109.5 . . ?
N8 B2 H2 109.1 . . ?
N8 B2 N10 109.8(7) . . ?
N8 B2 N12 108.5(6) . . ?
N10 B2 H2 109.1 . . ?
N10 B2 N12 111.0(7) . . ?
N12 B2 H2 109.1 . . ?
C2 C1 H1A 123.6 . . ?
N1 C1 H1A 123.6 . . ?
N1 C1 C2 112.7(8) . . ?
C4 N3 Sm1 131.0(6) . . ?
N4 N3 C4 103.9(7) . . ?
N4 N3 Sm1 123.8(5) . . ?
C1 C2 H2A 127.7 . . ?
C3 C2 C1 104.6(8) . . ?
C3 C2 H2A 127.7 . . ?
C2 C3 H3 125.3 . . ?
C2 C3 N2 109.5(7) . . ?
N2 C3 H3 125.3 . . ?
N3 C4 H4 124.9 . . ?
C5 C4 N3 110.3(9) . . ?
C5 C4 H4 124.9 . . ?
C10 N7 N8 105.4(6) . . ?
C10 N7 Sm2 131.9(6) . . ?
N8 N7 Sm2 122.6(4) . . ?
C5 C6 H6 126.5 . . ?
N4 C6 H6 126.5 . . ?
N4 C6 C5 107.1(8) . . ?
C8 C7 H7 124.8 . . ?
N5 C7 H7 124.8 . . ?
N5 C7 C8 110.4(7) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 C7 106.2(7) . . ?
C9 C8 H8 126.9 . . ?
C8 C9 H9 127.0 . . ?
C8 C9 N6 106.1(7) . . ?
N6 C9 H9 127.0 . . ?
N7 C10 H10 123.9 . . ?
N7 C10 C11 112.2(8) . . ?
C11 C10 H10 123.9 . . ?
C4 C5 C6 107.2(9) . . ?
C4 C5 H5 126.4 . . ?
C6 C5 H5 126.4 . . ?
C10 C11 H11 128.0 . . ?
C12 C11 C10 104.1(7) . . ?
C12 C11 H11 128.0 . . ?
C1 N1 Sm1 134.6(6) . . ?
C1 N1 N2 104.1(6) . . ?
N2 N1 Sm1 121.3(5) . . ?
C7 N5 Sm1 129.6(5) . . ?
C7 N5 N6 106.3(6) . . ?
N6 N5 Sm1 124.0(4) . . ?
N9 C13 H13 125.4 . . ?
N9 C13 C14 109.2(7) . . ?
C14 C13 H13 125.4 . . ?
C13 N9 N10 106.1(6) . . ?
C13 N9 Sm2 127.0(5) . . ?
N10 N9 Sm2 126.3(4) . . ?
C13 C14 H14 126.9 . . ?
C15 C14 C13 106.2(7) . . ?
C15 C14 H14 126.9 . . ?
C22 O1 Sm1 118.5(5) . . ?
C14 C15 H15 125.4 . . ?
N10 C15 C14 109.3(7) . . ?
N10 C15 H15 125.4 . . ?
N11 C16 H16 123.6 . . ?
N11 C16 C17 112.9(8) . . ?
C17 C16 H16 123.6 . . ?
C16 C17 H17 128.2 . . ?
C16 C17 C18 103.7(8) . . ?
C18 C17 H17 128.2 . . ?
C17 C18 H18 126.2 . . ?
N12 C18 C17 107.5(8) . . ?
N12 C18 H18 126.2 . . ?
O1 C22 C22 117.7(5) . 2_665 ?
O2 C22 O1 125.4(6) . . ?
O2 C22 C22 116.5(4) . 2_665 ?
N3 Sm1 N3 70.6(4) . 2_665 ?
N3 Sm1 N1 136.0(2) . 2_665 ?
N3 Sm1 N1 70.3(2) 2_665 2_665 ?
N3 Sm1 N1 70.3(2) . . ?
N3 Sm1 N1 136.0(2) 2_665 . ?
N1 Sm1 N1 152.9(3) . 2_665 ?
N5 Sm1 N3 77.2(2) 2_665 . ?
N5 Sm1 N3 76.3(2) 2_665 2_665 ?
N5 Sm1 N3 76.3(2) . . ?
N5 Sm1 N3 77.2(2) . 2_665 ?
N5 Sm1 N1 113.44(19) . 2_665 ?
N5 Sm1 N1 74.6(2) . . ?
N5 Sm1 N1 74.6(2) 2_665 2_665 ?
N5 Sm1 N1 113.44(19) 2_665 . ?
N5 Sm1 N5 147.3(3) 2_665 . ?
O1 Sm1 N3 145.4(2) 2_665 . ?
O1 Sm1 N3 145.4(2) . 2_665 ?
O1 Sm1 N3 122.2(2) 2_665 2_665 ?
O1 Sm1 N3 122.2(2) . . ?
O1 Sm1 N1 82.5(2) . 2_665 ?
O1 Sm1 N1 75.0(2) . . ?
O1 Sm1 N1 75.0(2) 2_665 2_665 ?
O1 Sm1 N1 82.5(2) 2_665 . ?
O1 Sm1 N5 76.18(19) 2_665 . ?
O1 Sm1 N5 135.0(2) . . ?
O1 Sm1 N5 76.18(19) . 2_665 ?
O1 Sm1 N5 135.0(2) 2_665 2_665 ?
O1 Sm1 O1 67.6(3) . 2_665 ?
C11 C12 H12 125.3 . . ?
N8 C12 C11 109.4(7) . . ?
N8 C12 H12 125.3 . . ?
C3 N2 B1 127.6(7) . . ?
C3 N2 N1 109.1(6) . . ?
N1 N2 B1 123.3(7) . . ?
N3 N4 B1 121.1(6) . . ?
N3 N4 C6 111.4(7) . . ?
C6 N4 B1 127.4(7) . . ?
C9 N6 B1 126.6(7) . . ?
N5 N6 B1 122.5(6) . . ?
N5 N6 C9 110.8(6) . . ?
N7 N8 B2 122.5(7) . . ?
C12 N8 B2 128.7(7) . . ?
C12 N8 N7 108.8(6) . . ?
N9 N10 B2 121.2(6) . . ?
C15 N10 B2 129.4(6) . . ?
C15 N10 N9 109.2(6) . . ?
N11 N12 B2 121.3(6) . . ?
C18 N12 N11 109.1(7) . . ?
C18 N12 B2 129.6(7) . . ?
C22 O2 Sm2 119.8(5) . . ?
N11 Sm2 N11 70.3(3) 2_665 . ?
N7 Sm2 N11 70.3(2) . . ?
N7 Sm2 N11 135.7(2) . 2_665 ?
N7 Sm2 N11 70.3(2) 2_665 2_665 ?
N7 Sm2 N11 135.7(2) 2_665 . ?
N7 Sm2 N7 153.2(3) . 2_665 ?
N9 Sm2 N11 74.9(2) . . ?
N9 Sm2 N11 74.9(2) 2_665 2_665 ?
N9 Sm2 N11 76.9(2) . 2_665 ?
N9 Sm2 N11 76.9(2) 2_665 . ?
N9 Sm2 N7 114.4(2) . 2_665 ?
N9 Sm2 N7 74.0(2) 2_665 2_665 ?
N9 Sm2 N7 114.4(2) 2_665 . ?
N9 Sm2 N7 74.0(2) . . ?
N9 Sm2 N9 145.3(3) . 2_665 ?
O2 Sm2 N11 145.4(2) . 2_665 ?
O2 Sm2 N11 145.4(2) 2_665 . ?
O2 Sm2 N11 123.0(2) 2_665 2_665 ?
O2 Sm2 N11 123.0(2) . . ?
O2 Sm2 N7 75.4(2) 2_665 2_665 ?
O2 Sm2 N7 82.2(2) . 2_665 ?
O2 Sm2 N7 82.2(2) 2_665 . ?
O2 Sm2 N7 75.4(2) . . ?
O2 Sm2 N9 135.3(2) . . ?
O2 Sm2 N9 77.8(2) . 2_665 ?
O2 Sm2 N9 77.8(2) 2_665 . ?
O2 Sm2 N9 135.3(2) 2_665 2_665 ?
O2 Sm2 O2 66.4(3) 2_665 . ?
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
N11 C16 1.297(11) . ?
N11 N12 1.379(9) . ?
N11 Sm2 2.592(7) . ?
B1 H1 1.0600 . ?
B1 N2 1.518(12) . ?
B1 N4 1.540(14) . ?
B1 N6 1.575(11) . ?
B2 H2 1.0600 . ?
B2 N8 1.526(12) . ?
B2 N10 1.531(10) . ?
B2 N12 1.542(11) . ?
C1 H1A 0.9500 . ?
C1 C2 1.367(13) . ?
C1 N1 1.344(11) . ?
N3 C4 1.398(11) . ?
N3 Sm1 2.538(7) . ?
N3 N4 1.339(10) . ?
C2 H2A 0.9500 . ?
C2 C3 1.343(11) . ?
C3 H3 0.9500 . ?
C3 N2 1.361(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.329(14) . ?
N7 C10 1.297(10) . ?
N7 N8 1.385(8) . ?
N7 Sm2 2.555(6) . ?
C6 H6 0.9500 . ?
C6 C5 1.365(14) . ?
C6 N4 1.346(10) . ?
C7 H7 0.9500 . ?
C7 C8 1.398(12) . ?
C7 N5 1.315(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.340(12) . ?
C9 H9 0.9500 . ?
C9 N6 1.383(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(13) . ?
C5 H5 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.357(11) . ?
N1 Sm1 2.558(7) . ?
N1 N2 1.371(9) . ?
N5 Sm1 2.504(6) . ?
N5 N6 1.328(8) . ?
C13 H13 0.9500 . ?
C13 N9 1.358(9) . ?
C13 C14 1.370(10) . ?
N9 N10 1.360(8) . ?
N9 Sm2 2.480(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.351(11) . ?
O1 C22 1.254(12) . ?
O1 Sm1 2.423(6) . ?
C15 H15 0.9500 . ?
C15 N10 1.331(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.336(14) . ?
C17 H17 0.9500 . ?
C17 C18 1.435(14) . ?
C18 H18 0.9500 . ?
C18 N12 1.310(10) . ?
C22 C22 1.529(13) 2_665 ?
C22 O2 1.248(13) . ?
C12 H12 0.9500 . ?
C12 N8 1.322(10) . ?
O2 Sm2 2.425(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 C16 C17 C18 3.0(14) . . . . ?
C1 C2 C3 N2 -0.2(10) . . . . ?
C1 N1 N2 B1 179.5(7) . . . . ?
C1 N1 N2 C3 0.7(8) . . . . ?
N3 C4 C5 C6 2.7(13) . . . . ?
C2 C1 N1 Sm1 177.8(6) . . . . ?
C2 C1 N1 N2 -0.9(9) . . . . ?
C2 C3 N2 B1 -179.0(8) . . . . ?
C2 C3 N2 N1 -0.3(9) . . . . ?
C4 N3 N4 B1 179.3(8) . . . . ?
C4 N3 N4 C6 -0.9(10) . . . . ?
N7 C10 C11 C12 1.4(11) . . . . ?
C7 C8 C9 N6 -3.2(10) . . . . ?
C7 N5 N6 B1 -177.7(8) . . . . ?
C7 N5 N6 C9 -1.4(9) . . . . ?
C8 C7 N5 Sm1 -178.8(5) . . . . ?
C8 C7 N5 N6 -0.7(10) . . . . ?
C8 C9 N6 B1 179.1(8) . . . . ?
C8 C9 N6 N5 3.0(10) . . . . ?
C10 N7 N8 B2 -175.3(7) . . . . ?
C10 N7 N8 C12 3.0(8) . . . . ?
C10 C11 C12 N8 0.6(10) . . . . ?
C5 C6 N4 B1 -177.7(9) . . . . ?
C5 C6 N4 N3 2.6(10) . . . . ?
C11 C12 N8 B2 176.0(7) . . . . ?
C11 C12 N8 N7 -2.3(9) . . . . ?
N1 C1 C2 C3 0.7(10) . . . . ?
N5 C7 C8 C9 2.5(11) . . . . ?
C13 N9 N10 B2 -173.0(7) . . . . ?
C13 N9 N10 C15 2.0(8) . . . . ?
C13 C14 C15 N10 0.2(9) . . . . ?
N9 C13 C14 C15 1.1(9) . . . . ?
C14 C13 N9 N10 -1.9(8) . . . . ?
C14 C13 N9 Sm2 -173.2(5) . . . . ?
C14 C15 N10 B2 173.1(8) . . . . ?
C14 C15 N10 N9 -1.4(8) . . . . ?
O1 C22 O2 Sm2 178.8(5) . . . . ?
C16 N11 N12 B2 179.2(8) . . . . ?
C16 N11 N12 C18 -2.0(10) . . . . ?
C16 C17 C18 N12 -4.1(14) . . . . ?
C17 C18 N12 N11 3.8(12) . . . . ?
C17 C18 N12 B2 -177.6(9) . . . . ?
C22 C22 O2 Sm2 -8.7(10) 2_665 . . . ?
Sm1 N3 C4 C5 -167.8(7) . . . . ?
Sm1 N3 N4 B1 -12.7(10) . . . . ?
Sm1 N3 N4 C6 167.0(5) . . . . ?
Sm1 N1 N2 B1 0.6(9) . . . . ?
Sm1 N1 N2 C3 -178.2(5) . . . . ?
Sm1 N5 N6 B1 0.5(10) . . . . ?
Sm1 N5 N6 C9 176.9(5) . . . . ?
Sm1 O1 C22 C22 1.6(9) . . . 2_665 ?
Sm1 O1 C22 O2 174.0(6) . . . . ?
N2 B1 N4 N3 -53.9(10) . . . . ?
N2 B1 N4 C6 126.4(8) . . . . ?
N2 B1 N6 C9 -116.2(9) . . . . ?
N2 B1 N6 N5 59.6(10) . . . . ?
N4 B1 N2 C3 -120.4(8) . . . . ?
N4 B1 N2 N1 61.0(9) . . . . ?
N4 B1 N6 C9 124.6(9) . . . . ?
N4 B1 N6 N5 -59.6(9) . . . . ?
N4 N3 C4 C5 -1.1(12) . . . . ?
N4 C6 C5 C4 -3.2(12) . . . . ?
N6 B1 N2 C3 119.4(8) . . . . ?
N6 B1 N2 N1 -59.1(10) . . . . ?
N6 B1 N4 N3 66.2(9) . . . . ?
N6 B1 N4 C6 -113.5(9) . . . . ?
N8 B2 N10 N9 60.7(9) . . . . ?
N8 B2 N10 C15 -113.2(8) . . . . ?
N8 B2 N12 N11 -56.2(10) . . . . ?
N8 B2 N12 C18 125.4(10) . . . . ?
N8 N7 C10 C11 -2.7(10) . . . . ?
N10 B2 N8 N7 -60.6(9) . . . . ?
N10 B2 N8 C12 121.4(8) . . . . ?
N10 B2 N12 N11 64.6(9) . . . . ?
N10 B2 N12 C18 -113.8(11) . . . . ?
N12 N11 C16 C17 -0.8(13) . . . . ?
N12 B2 N8 N7 60.9(9) . . . . ?
N12 B2 N8 C12 -117.1(8) . . . . ?
N12 B2 N10 N9 -59.3(9) . . . . ?
N12 B2 N10 C15 126.8(8) . . . . ?
Sm2 N11 C16 C17 -171.2(8) . . . . ?
Sm2 N11 N12 B2 -9.4(10) . . . . ?
Sm2 N11 N12 C18 169.3(7) . . . . ?
Sm2 N7 C10 C11 179.4(6) . . . . ?
Sm2 N7 N8 B2 2.8(8) . . . . ?
Sm2 N7 N8 C12 -178.9(5) . . . . ?
Sm2 N9 N10 B2 -1.6(9) . . . . ?
Sm2 N9 N10 C15 173.4(5) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.72(3)
2 0.28(3)
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.393 -0.021 -0.812 4473.8 1029.1 ?
