Di- and tetranuclear transition metal complexes of a tetrakisguanidino-substituted phenazine dye by stepwise coordination.
Lorenz, Roxana; Kaifer, Elisabeth; Wadepohl, Hubert; Himmel, Hans-Jörg; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11016–11029; doi:10.1039/c8dt02176g

data_7047000
_publ_section_title
;
 Di- and tetranuclear transition metal complexes of a
 tetrakisguanidino-substituted phenazine dye by stepwise coordination.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11016
_journal_page_last               11029
_journal_paper_doi               10.1039/c8dt02176g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C35.5 H59 Cl11 Cu2 N14'
_chemical_formula_weight         1198.99
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_rl1
_audit_creation_date             2016-03-31
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.0818(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.8999(4)
_cell_length_b                   14.17669(13)
_cell_length_c                   24.7543(3)
_cell_measurement_reflns_used    29937
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.4750
_cell_measurement_theta_min      3.2990
_cell_volume                     10698.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -43.00  57.00   0.50   17.50    --   26.87 -77.00  30.00  200
  2  \w      6.00  96.00   0.50   17.50    --   26.87  57.00 150.00  180
  3  \w    -20.00  69.00   0.50   17.50    --   26.87 -99.00-120.00  178
  4  \w     52.00  96.00   0.50   17.50    --   26.87  57.00 -90.00   88
  5  \w    -42.00  41.00   0.50   17.50    --   26.87 -57.00 120.00  166
  6  \w    -46.00  34.00   0.50   17.50    --   26.87 -38.00-120.00  160
  7  \w     -2.00  84.00   0.50   17.50    --   26.87  77.00  30.00  172
  8  \w     35.00  61.00   0.50   17.50    --   26.87  57.00-150.00   52
  9  \w    -20.00  69.00   0.50   17.50    --   26.87 -99.00   0.00  178
 10  \w      4.00  33.00   0.50   17.50    --   26.87  77.00 -60.00   58
 11  \w    -17.00  15.00   0.50   17.50    --   26.87 -99.00  90.00   64
 12  \w     31.00  69.00   0.50   17.50    --   26.87 -99.00  90.00   76
 13  \w      2.00  91.00   0.50   17.50    --   26.87  38.00  30.00  178
 14  \w      3.00  29.00   0.50   17.50    --   26.87  77.00 120.00   52
 15  \w      0.00  97.00   0.50   17.50    --   26.87  77.00-150.00  194
 16  \w     11.00  54.00   0.50   17.50    --   26.87  45.00-132.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0114555000
_diffrn_orient_matrix_UB_12      0.0434286000
_diffrn_orient_matrix_UB_13      0.0073613000
_diffrn_orient_matrix_UB_21      -0.0060450000
_diffrn_orient_matrix_UB_22      0.0042186000
_diffrn_orient_matrix_UB_23      0.0245470000
_diffrn_orient_matrix_UB_31      0.0193330000
_diffrn_orient_matrix_UB_32      -0.0244523000
_diffrn_orient_matrix_UB_33      0.0173115000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            133467
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.008
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.386
_exptl_absorpt_correction_T_max  0.87620
_exptl_absorpt_correction_T_min  0.87620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4920
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         16336
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      7.745
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0489P)^2^+17.9394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13017
_reflns_number_total             16336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02176g2.cif
_cod_data_source_block           hi_rl1_sq
_cod_depositor_comments
'Adding full bibliography for 7047000--7047008.cif.'
_cod_original_formula_sum        'C35.50 H59 Cl11 Cu2 N14'
_cod_database_code               7047000
_audit_block_refno               2687
_audit_block_usercomment         'gu07KS2, irregular, black'
_chemical_oxdiff_formula         'C36 H54 Cl10 Cu2 N14'
_chemical_oxdiff_usercomment     'gu07KS2, irregular, black'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.874
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_shelxl_version_number           2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-Cl1 \\sim C51-Cl52 \\sim C61-Cl61 \\sim C61-Cl62 \\sim C71_$1-Cl71_$1
\\sim C71_$1-Cl72_$1 ~
 C71_$1-Cl73_$1 \\sim C71_$1-Cl74_$1
 with sigma of 0.02
 Cl51-Cl52 \\sim Cl61-Cl62 \\sim Cl71_$1-Cl72_$1 \\sim Cl73_$1-Cl74_$1
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl71, C71, Cl72, Cl73, Cl74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H71A)=Sof(H71B)=Sof(Cl73)=Sof(Cl74)=1-FVAR(1)
 Sof(Cl71)=Sof(H71C)=Sof(H71D)=Sof(Cl72)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71C,H71D), C71(H71A,H71B), C51(H51A,H51B), C61(H61A,H61B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C19(H19), C22(H22)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), 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)
;
_shelx_fab_checksum              41301
_platon_squeeze_void_probe_radius 1.20
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.860
_shelx_res_checksum              43553
_cell_oxdiff_length_a            32.8944(4)
_cell_oxdiff_length_b            14.18103(17)
_cell_oxdiff_length_c            24.7519(3)
_cell_oxdiff_angle_alpha         90.0123(10)
_cell_oxdiff_angle_beta          112.0884(11)
_cell_oxdiff_angle_gamma         89.9616(10)
_cell_oxdiff_volume              10698.8(2)
_cell_oxdiff_measurement_reflns_used 29937