On the metal-ligand bonding in dinuclear complexes with redox-active guanidine ligands.
Steuer, Lena; Kaifer, Elisabeth; Himmel, Hans-Jörg; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9467–9482; doi:10.1039/d1dt01354h

data_7707633
_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 H52 Cl4 Mn2 N12 O2, 0.5(C4 H8 O), 0.25(C3 H7 N O)'
_chemical_formula_sum            'C34.75 H57.75 Cl4 Mn2 N12.25 O2.75'
_chemical_formula_weight         942.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-12
_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                 101.510(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6798(6)
_cell_length_b                   18.3575(9)
_cell_length_c                   18.5402(10)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.24
_cell_volume                     4562.3(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2018.7-2 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon III detector'
_diffrn_detector_type            'CPAD detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\w and \f 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  0.0655
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            128807
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.746
_diffrn_reflns_theta_min         2.029
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1592 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.9515.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         11812
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0360
_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/[\s^2^(Fo^2^)+(0.0482P)^2^+3.4980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9761
_reflns_number_total             11812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01354h2.cif
_cod_data_source_block           mo_ls311_01
_cod_depositor_comments
'Adding full bibliography for 7707623--7707635.cif.'
_cod_database_code               7707633
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45-O4
 1.22 with sigma of 0.02
 C45-N13
 1.36 with sigma of 0.02
 N13-C46
 1.45 with sigma of 0.02
 N13-C47
 1.46 with sigma of 0.02
 C45-C46
 2.46 with sigma of 0.04
 C45-C47
 2.45 with sigma of 0.04
 N13-C46 \\sim N13-C47
 with sigma of 0.02
3. Restrained planarity
 O4, N13, C45, C46, C47
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O4 \\sim N13 \\sim C45 \\sim C46 \\sim C47: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O4, N13, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O3(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42(0.5)
 C43(0.5) H43(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) O4(0.25) N13(0.25)
 C45(0.25) H45(0.25) C46(0.25) H46A(0.25) H46B(0.25) H46C(0.25) C47(0.25)
 H47A(0.25) H47B(0.25) H47C(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C12(H12), C42(H42), C43(H43), C45(H45)
7.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              66962
_shelx_hkl_checksum              27169
_olex2_submission_special_instructions 'No special instructions were received'