#------------------------------------------------------------------------------
#$Date: 2021-09-06 13:58:25 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/76/7707630.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_7707630
loop_
_publ_author_name
'Steuer, Lena'
'Kaifer, Elisabeth'
'Himmel, Hans-Jörg'
_publ_section_title
;
 On the metal-ligand bonding in dinuclear complexes with redox-active
 guanidine ligands.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9467
_journal_page_last               9482
_journal_paper_doi               10.1039/d1dt01354h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C32 H44 N12 O2'
_chemical_formula_sum            'C32 H44 N12 O2'
_chemical_formula_weight         628.79
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.574(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7374(11)
_cell_length_b                   13.3856(17)
_cell_length_c                   15.6864(18)
_cell_measurement_reflns_used    8990
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.62
_cell_volume                     1610.5(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 v2018.7-2 (Bruker AX'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CPAD detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_unetI/netI     0.0986
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20467
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         2.007
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5903
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1050 before and 0.0647 after correction. The Ratio of minimum to maximum transmission is 0.7912. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0577
_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)+(0.0457P)²+0.2075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2490
_reflns_number_total             4080
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01354h2.cif
_cod_data_source_block           2019_ls146_1
_cod_depositor_comments
'Adding full bibliography for 7707623--7707635.cif.'
_cod_database_code               7707630
_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.
;
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C13(H13a,H13b), C14(H14a,H14b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
2.c Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
O1 O 0.34178(16) 0.55715(9) 0.48070(9) 0.0248(3) Uani 1 1 d . . . . .
N1 N 0.6211(2) 0.84316(12) 0.61439(10) 0.0231(4) Uani 1 1 d . . . . .
N2 N 0.6435(2) 0.99172(12) 0.69031(11) 0.0261(4) Uani 1 1 d . . . . .
N3 N 0.6876(2) 0.85305(13) 0.76994(10) 0.0260(4) Uani 1 1 d . . . . .
N4 N 0.06685(19) 0.28234(12) 0.32446(10) 0.0242(4) Uani 1 1 d . . . . .
N5 N -0.0210(2) 0.14723(12) 0.41201(11) 0.0267(4) Uani 1 1 d . . . . .
N6 N -0.1475(2) 0.16618(13) 0.27613(11) 0.0270(4) Uani 1 1 d . . . . .
C1 C 0.6335(2) 0.74064(14) 0.59990(12) 0.0212(4) Uani 1 1 d . . . . .
C2 C 0.2123(2) 0.31680(14) 0.37937(12) 0.0215(4) Uani 1 1 d . . . . .
C3 C 0.2120(2) 0.41601(14) 0.40679(12) 0.0224(4) Uani 1 1 d . . . . .
H3 H 0.109580 0.454935 0.392560 0.027 Uiso 1 1 calc R . . . .
C4 C 0.3556(2) 0.45918(14) 0.45383(12) 0.0203(4) Uani 1 1 d . . . . .
C5 C 0.4932(2) 0.59652(14) 0.52626(12) 0.0201(4) Uani 1 1 d . . . . .
C6 C 0.4892(2) 0.69472(14) 0.55197(12) 0.0213(4) Uani 1 1 d . . . . .
H6 H 0.385797 0.732492 0.536815 0.026 Uiso 1 1 calc R . . . .
C7 C 0.6511(2) 0.88826(15) 0.68697(13) 0.0223(4) Uani 1 1 d . . . . .
C8 C 0.7160(3) 1.02571(17) 0.77606(14) 0.0337(5) Uani 1 1 d . . . . .
H8A H 0.654752 1.085840 0.793386 0.040 Uiso 1 1 calc R . . . .
H8B H 0.842194 1.040123 0.779461 0.040 Uiso 1 1 calc R . . . .
C9 C 0.6823(3) 0.93639(17) 0.82999(14) 0.0348(5) Uani 1 1 d . . . . .
H9A H 0.773745 0.929467 0.880091 0.042 Uiso 1 1 calc R . . . .
H9B H 0.567008 0.941151 0.850552 0.042 Uiso 1 1 calc R . . . .
C10 C 0.6729(3) 1.05013(16) 0.61624(15) 0.0373(6) Uani 1 1 d . . . . .
H10A H 0.797643 1.050261 0.610746 0.056 Uiso 1 1 calc GR . . . .
H10B H 0.633459 1.118850 0.623264 0.056 Uiso 1 1 calc GR . . . .
H10C H 0.607681 1.020948 0.564404 0.056 Uiso 1 1 calc GR . . . .
C11 C 0.6246(3) 0.75686(16) 0.79468(13) 0.0331(5) Uani 1 1 d . . . . .
H11A H 0.500516 0.750416 0.772754 0.050 Uiso 1 1 calc GR . . . .
H11B H 0.640432 0.751458 0.857528 0.050 Uiso 1 1 calc GR . . . .
H11C H 0.690167 0.703594 0.770492 0.050 Uiso 1 1 calc GR . . . .
C12 C -0.0226(2) 0.20423(15) 0.33900(13) 0.0230(4) Uani 1 1 d . . . . .
C13 C -0.1673(3) 0.07674(16) 0.39912(15) 0.0324(5) Uani 1 1 d . . . . .
H13A H -0.271876 0.104040 0.421017 0.039 Uiso 1 1 calc R . . . .
H13B H -0.136242 0.011801 0.427262 0.039 Uiso 1 1 calc R . . . .
C14 C -0.1950(3) 0.06697(16) 0.30253(15) 0.0327(5) Uani 1 1 d . . . . .
H14A H -0.118328 0.015128 0.282608 0.039 Uiso 1 1 calc R . . . .
H14B H -0.317980 0.051121 0.280906 0.039 Uiso 1 1 calc R . . . .
C15 C 0.0261(3) 0.19079(17) 0.49686(14) 0.0352(5) Uani 1 1 d . . . . .
H15A H 0.153008 0.198490 0.508277 0.053 Uiso 1 1 calc GR . . . .
H15B H -0.013474 0.146883 0.540380 0.053 Uiso 1 1 calc GR . . . .
H15C H -0.029493 0.256356 0.499085 0.053 Uiso 1 1 calc GR . . . .
C16 C -0.1333(3) 0.18454(17) 0.18643(14) 0.0338(5) Uani 1 1 d . . . . .
H16A H -0.102837 0.254731 0.178719 0.051 Uiso 1 1 calc GR . . . .
H16B H -0.244977 0.169754 0.151597 0.051 Uiso 1 1 calc GR . . . .
H16C H -0.042330 0.141568 0.168230 0.051 Uiso 1 1 calc GR . . . .
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'
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
C4 O1 C5 114.88(14) . . ?
C7 N1 C1 126.79(18) . . ?
C7 N2 C8 109.44(17) . . ?
C7 N2 C10 119.89(16) . . ?
C10 N2 C8 119.39(18) . . ?
C7 N3 C9 109.10(17) . . ?
C7 N3 C11 121.52(17) . . ?
C11 N3 C9 117.79(16) . . ?
C12 N4 C2 124.30(17) . . ?
C12 N5 C13 108.67(17) . . ?
C12 N5 C15 120.89(17) . . ?
C15 N5 C13 118.66(16) . . ?
C12 N6 C14 108.21(17) . . ?
C12 N6 C16 119.66(16) . . ?
C16 N6 C14 119.15(17) . . ?
N1 C1 C2 124.64(17) . 3_666 ?
N1 C1 C6 116.81(17) . . ?
C6 C1 C2 118.06(17) . 3_666 ?
N4 C2 C1 122.99(16) . 3_666 ?
C3 C2 N4 117.92(17) . . ?
C3 C2 C1 118.69(17) . 3_666 ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122.01(18) . . ?
C4 C3 H3 119.0 . . ?
O1 C4 C5 122.43(17) . 3_666 ?
C3 C4 O1 118.09(16) . . ?
C3 C4 C5 119.47(17) . 3_666 ?
C4 C5 O1 122.64(17) 3_666 . ?
C6 C5 O1 117.51(16) . . ?
C6 C5 C4 119.85(17) . 3_666 ?
C1 C6 H6 119.0 . . ?
C5 C6 C1 121.91(17) . . ?
C5 C6 H6 119.0 . . ?
N1 C7 N2 119.99(18) . . ?
N1 C7 N3 131.91(18) . . ?
N3 C7 N2 108.07(16) . . ?
N2 C8 H8A 111.5 . . ?
N2 C8 H8B 111.5 . . ?
N2 C8 C9 101.31(17) . . ?
H8A C8 H8B 109.3 . . ?
C9 C8 H8A 111.5 . . ?
C9 C8 H8B 111.5 . . ?
N3 C9 C8 102.82(16) . . ?
N3 C9 H9A 111.2 . . ?
N3 C9 H9B 111.2 . . ?
C8 C9 H9A 111.2 . . ?
C8 C9 H9B 111.2 . . ?
H9A C9 H9B 109.1 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 N5 130.60(19) . . ?
N4 C12 N6 120.84(18) . . ?
N5 C12 N6 108.55(16) . . ?
N5 C13 H13A 111.5 . . ?
N5 C13 H13B 111.5 . . ?
N5 C13 C14 101.51(16) . . ?
H13A C13 H13B 109.3 . . ?
C14 C13 H13A 111.5 . . ?
C14 C13 H13B 111.5 . . ?
N6 C14 C13 101.49(16) . . ?
N6 C14 H14A 111.5 . . ?
N6 C14 H14B 111.5 . . ?
C13 C14 H14A 111.5 . . ?
C13 C14 H14B 111.5 . . ?
H14A C14 H14B 109.3 . . ?
N5 C15 H15A 109.5 . . ?
N5 C15 H15B 109.5 . . ?
N5 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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
O1 C4 1.386(2) . ?
O1 C5 1.393(2) . ?
N1 C1 1.396(2) . ?
N1 C7 1.282(2) . ?
N2 C7 1.387(3) . ?
N2 C8 1.460(3) . ?
N2 C10 1.443(3) . ?
N3 C7 1.378(3) . ?
N3 C9 1.464(3) . ?
N3 C11 1.448(3) . ?
N4 C2 1.402(2) . ?
N4 C12 1.291(2) . ?
N5 C12 1.375(3) . ?
N5 C13 1.467(2) . ?
N5 C15 1.455(3) . ?
N6 C12 1.384(2) . ?
N6 C14 1.453(3) . ?
N6 C16 1.447(3) . ?
C1 C2 1.420(3) 3_666 ?
C1 C6 1.403(3) . ?
C2 C3 1.396(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(3) . ?
C4 C5 1.388(3) 3_666 ?
C5 C6 1.376(3) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.507(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.508(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
