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_7033231
_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 Cu N6 O5, 2(B F4), 2(H2 O)'
_chemical_formula_sum            'C33 H38 B2 Cu F8 N6 O7'
_chemical_formula_weight         867.85
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_hr23
_audit_creation_date
;
'Sat Jun 29 18:19:10 2013'
;
_audit_update_record             'Thu Jul 24 16:05:11 CEST 2014'
_cell_angle_alpha                90
_cell_angle_beta                 103.2779(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7553(3)
_cell_length_b                   10.30900(12)
_cell_length_c                   17.8036(2)
_cell_measurement_reflns_used    17472
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      25.5370
_cell_measurement_theta_min      3.5740
_cell_volume                     3707.54(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   12.00   48.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8347   77.0000  120.0000 72

  2 omega  -50.00  -23.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8347   79.0000  -39.8201 54

  3 omega  -50.00  -19.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8347   79.0000  -71.4302 62

  4 omega  -48.00  -23.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8347   77.0000  120.0000 50

  5 omega  -50.00   11.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8347   79.0000   29.1181 122

  6 omega  -12.00   87.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   77.0000  120.0000 198

  7 omega   25.00   50.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -80.0000  -81.6192 50

  8 omega  -20.00   50.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -79.0000 -168.4484 140

  9 omega  -51.00   14.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -57.0000  -30.0000 130

 10 omega    5.00   76.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000 -120.0000 142

 11 omega  -46.00   -1.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -80.0000  -81.6192 90

 12 omega   11.00   77.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000   30.0000 132

 13 omega  -15.00   10.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   77.0000   30.0000 50

 14 omega   61.00   88.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   77.0000   30.0000 54

 15 omega  -47.00   48.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -77.0000   90.0000 190

 16 omega   10.00   79.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000  -60.0000 138

 17 omega  -52.00   38.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -57.0000  150.0000 180

 18 omega  -52.00   38.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -57.0000  -30.0000 180

 19 omega   -5.00   86.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000   90.0000 182

 20 omega  -11.00   16.50   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   38.0000  -60.0000 55

;
_diffrn_measurement_device       '\k-geometry 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_UB_11      -0.0350327000
_diffrn_orient_matrix_UB_12      -0.0027705000
_diffrn_orient_matrix_UB_13      -0.0071559000
_diffrn_orient_matrix_UB_21      0.0004279000
_diffrn_orient_matrix_UB_22      -0.0615215000
_diffrn_orient_matrix_UB_23      -0.0177036000
_diffrn_orient_matrix_UB_31      0.0023769000
_diffrn_orient_matrix_UB_32      -0.0306547000
_diffrn_orient_matrix_UB_33      0.0362050000
_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  0.0649
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            70356
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.695
_diffrn_reflns_theta_min         3.232
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       plate
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7025
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0386P)^2^+6.5101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5859
_reflns_number_total             7025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03262d2.cif
_cod_data_source_block           co_hr23
_cod_depositor_comments
'Adding full bibliography for 7033230--7033235.cif.'
_cod_original_cell_volume        3707.55(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7033231
_audit_block_refno               1787
_audit_block_usercomment         'HR288, plate, blue'
_chemical_oxdiff_formula         'C33 H38 N6 O7 Cu B2 F8'
_chemical_oxdiff_usercomment     'HR288, plate, blue'
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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 1.3 times of:
  All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Same fragment restrains
{F12, F11, F13, F14, B1}
as
{F21, F22, F23, F24, B2}
3.a Free rotating group:
 O77(H77A,H77B), O78(H78A,H78B)
3.b Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C25(H25)
3.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B)
3.d 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)
3.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C)
3.f Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              54887
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            20.7503(4)
_cell_oxdiff_length_b            10.31085(19)
_cell_oxdiff_length_c            17.8019(2)
_cell_oxdiff_angle_alpha         89.9936(13)
_cell_oxdiff_angle_beta          103.2388(15)
_cell_oxdiff_angle_gamma         89.9522(16)
_cell_oxdiff_volume              3707.55(11)
_cell_oxdiff_measurement_reflns_used 17472