Synthesis and transition metal coordination chemistry of a novel hexadentate bispidine ligand.
Comba, Peter; Rudolf, Henning; Wadepohl, Hubert; Dalton transactions (Cambridge, England : 2003) 44 (2015) 2724–2736; doi:10.1039/c4dt03262d

data_7033234
_publ_section_title
;
 Synthesis and transition metal coordination chemistry of a novel
 hexadentate bispidine ligand.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2724
_journal_page_last               2736
_journal_paper_doi               10.1039/c4dt03262d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C33 H34 Cl Fe N6 O5, Cl1'
_chemical_formula_sum            'C33 H34 Cl2 Fe N6 O5'
_chemical_formula_weight         720.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_hr6
_audit_creation_date
;
'Fri May 11 16:22:32 2012'
;
_audit_update_record             'Thu Jul 24 16:55:04 CEST 2014'
_cell_angle_alpha                79.632(2)
_cell_angle_beta                 84.430(2)
_cell_angle_gamma                76.8063(18)
_cell_formula_units_Z            2
_cell_length_a                   8.40726(19)
_cell_length_b                   14.6959(3)
_cell_length_c                   15.2169(4)
_cell_measurement_reflns_used    23818
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      29.8144
_cell_measurement_theta_min      3.2796
_cell_volume                     1797.49(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega   25.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -77.0000  -90.0000 26

  2 omega  -10.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224   77.0000   60.0000 101

  3 omega  -50.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -77.0000   30.0000 101

  4 omega  -10.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224   77.0000  -60.0000 101

  5 omega    1.00   83.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224   57.0000 -180.0000 82

  6 omega  -29.00   10.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -57.0000 -150.0000 39

  7 phi    269.00  310.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
  20.5224   20.5224   40.0000     -     41

  8 omega  -42.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -77.0000  -60.0000 93

  9 omega  -42.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -77.0000 -180.0000 93

 10 omega  -73.00  -46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912  -57.0000  120.0000 27

 11 omega  -51.00  -24.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   77.0000 -150.0000 27

 12 omega  -74.00  -47.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912  -57.0000    0.0000 27

 13 omega  -51.00  -24.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   77.0000   60.0000 27

 14 omega    6.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   77.0000   60.0000 43

 15 omega  -51.00    3.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   77.0000  120.0000 54

 16 omega  -25.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912  -57.0000  120.0000 25

 17 omega  -52.00  -26.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   78.0000  -77.0000 26

 18 omega   -1.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224   57.0000 -180.0000 90

 19 omega  -48.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -57.0000  -90.0000 90

 20 omega  -50.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -77.0000   90.0000 101

 21 omega  -48.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -57.0000 -150.0000 90

 22 omega  -10.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224   77.0000 -150.0000 101

 23 omega  -50.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -77.0000  -90.0000 101

 24 omega   -1.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224   57.0000  -30.0000 90

 25 omega  -48.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224  -57.0000  -60.0000 90

 26 omega  -24.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5224   19.0000   60.0000 117

 27 omega  -51.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   77.0000  -60.0000 100

 28 omega  -90.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912  -57.0000  120.0000 90

 29 omega  -52.00   28.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   78.0000  -77.0000 80

 30 omega  -51.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   77.0000 -180.0000 100

 31 omega  -46.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   38.0000 -180.0000 97

 32 omega  -94.00   52.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912    0.0000    0.0000 146

 33 omega  -94.00   19.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912    0.0000  120.0000 113

 34 omega  -51.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9912   77.0000   30.0000 100

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0009828000
_diffrn_orient_matrix_UB_12      0.0103474000
_diffrn_orient_matrix_UB_13      -0.0473321000
_diffrn_orient_matrix_UB_21      0.0631952000
_diffrn_orient_matrix_UB_22      0.0251055000
_diffrn_orient_matrix_UB_23      -0.0014692000
_diffrn_orient_matrix_UB_31      0.0594999000
_diffrn_orient_matrix_UB_32      -0.0422748000
_diffrn_orient_matrix_UB_33      -0.0032697000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            97442
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.881
_diffrn_reflns_theta_min         3.286
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       needle
_exptl_crystal_F_000             747
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         9872
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0659
_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/[\s^2^(Fo^2^)+(0.0289P)^2^+3.7554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8736
_reflns_number_total             9872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03262d2.cif
_cod_data_source_block           co_hr6
_cod_depositor_comments
'Adding full bibliography for 7033230--7033235.cif.'
_cod_original_cell_volume        1797.48(8)
_cod_database_code               7033234
_audit_block_refno               1497
_audit_block_usercomment         'HR358, needle, yellow'
_chemical_oxdiff_formula         'C33 H34 Cl2 Fe1 N6 O5'
_chemical_oxdiff_usercomment     'HR358, needle, yellow'
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.941
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_shelxl_version_number           2014-3
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl4: within 1A with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 1*[Sof(Cl2)]+1*[Sof(Cl3)]+1*[Sof(Cl4)]=1 with esd of 0.01
4.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C25(H25)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
 C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
  C35(H35)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C)
4.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_smtbx_masks_special_details
;
The smtbx solvent masking procedure was used to remove the
electronic contribution of solvent molecules from the F(obs).
(P. v. d. Sluis, A. L. Spek, Acta Cryst. 1990, A46, 194; http://cctbx.sourceforge.net)
;
_shelx_res_checksum              67907
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            8.40726(19)
_cell_oxdiff_length_b            14.6959(3)
_cell_oxdiff_length_c            15.2169(4)
_cell_oxdiff_angle_alpha         79.632(2)
_cell_oxdiff_angle_beta          84.430(2)
_cell_oxdiff_angle_gamma         76.8063(18)
_cell_oxdiff_volume              1797.48(7)
_cell_oxdiff_measurement_reflns_used 23818