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_7047007
_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_moiety         'C36 H58 Cl6 Cu2 N16 Ni2'
_chemical_formula_sum            'C36 H58 Cl6 Cu2 N16 Ni2'
_chemical_formula_weight         1172.18
_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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_rl4
_audit_creation_date             2017-05-10
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.7608(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4307(2)
_cell_length_b                   13.47874(19)
_cell_length_c                   15.9132(3)
_cell_measurement_reflns_used    18152
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.0110
_cell_measurement_theta_min      2.6610
_cell_volume                     2552.99(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 1.000
_diffrn_measured_fraction_theta_max 0.970
_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      7.00  96.00   0.50   15.00    --   27.02  57.00-120.00  178
  2  \w    -20.00  69.00   0.50   15.00    --   27.02 -99.00 -60.00  178
  3  \w    -42.00  48.00   0.50   15.00    --   27.02 -57.00   0.00  180
  4  \w    -42.00  48.00   0.50   15.00    --   27.02 -57.00-180.00  180
  5  \w      7.00  96.00   0.50   15.00    --   27.02  57.00 -30.00  178
  6  \w     -3.00  97.00   0.50   15.00    --   27.02  77.00 150.00  200
  7  \w    -20.00  69.00   0.50   15.00    --   27.02 -99.00 120.00  178
  8  \w     -3.00  97.00   0.50   15.00    --   27.02  77.00  60.00  200
  9  \w     -3.00  97.00   0.50   15.00    --   27.02  77.00 -90.00  200
 10  \w      7.00  96.00   0.50   15.00    --   27.02  57.00  30.00  178
 11  \w    -42.00  48.00   0.50   15.00    --   27.02 -57.00  90.00  180
 12  \w    -20.00  69.00   0.50   15.00    --   27.02 -99.00   0.00  178
 13  \w    -20.00  16.00   0.50   15.00    --   27.02 -99.00-120.00   72
 14  \w      2.00  99.00   0.50   15.00    --   27.02  38.00 150.00  194
;
_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      0.0588088000
_diffrn_orient_matrix_UB_12      0.0016407000
_diffrn_orient_matrix_UB_13      0.0061524000
_diffrn_orient_matrix_UB_21      0.0038540000
_diffrn_orient_matrix_UB_22      -0.0513186000
_diffrn_orient_matrix_UB_23      0.0103319000
_diffrn_orient_matrix_UB_31      -0.0088808000
_diffrn_orient_matrix_UB_32      -0.0115593000
_diffrn_orient_matrix_UB_33      -0.0449635000
_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  0.0715
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78702
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.402
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         8896
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+2.3727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6911
_reflns_number_total             8896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02176g2.cif
_cod_data_source_block           hi_rl4
_cod_depositor_comments
'Adding full bibliography for 7047000--7047008.cif.'
_cod_database_code               7047007
_audit_block_refno               2879
_audit_block_usercomment         'rlfp05b, plate, dark red'
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.832
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_shelxl_version_number           2017/1
_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
 Ni-Cl2A \\sim Ni-Cl2B
 with sigma of 0.02
3. Others
 Sof(Cl2B)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
4.b 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), C18(H18A,H18B,H18C)
;
_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 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.779
_shelx_res_checksum              38578
_cell_oxdiff_length_a            12.4303(4)
_cell_oxdiff_length_b            13.4771(2)
_cell_oxdiff_length_c            15.9174(5)
_cell_oxdiff_angle_alpha         89.983(2)
_cell_oxdiff_angle_beta          106.782(3)
_cell_oxdiff_angle_gamma         90.029(2)
_cell_oxdiff_volume              2552.99(13)
_cell_oxdiff_measurement_reflns_used 18152