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_7033232
_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
'C34.68 H38.73 Fe N6 O6.68, 2(B F4), C4 H10 O'
_chemical_formula_sum            'C38.68 H48.73 B2 F8 Fe N6 O7.68'
_chemical_formula_weight         950.18
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_hr8
_audit_creation_date             2013-07-17
_audit_update_record             'Wed Jul 17 15:50:07 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 99.311(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.538(5)
_cell_length_b                   15.040(7)
_cell_length_c                   27.068(14)
_cell_measurement_reflns_used    7602
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.93
_cell_measurement_theta_min      2.21
_cell_volume                     4234(4)
_computing_cell_refinement
;
SAINT 8.x (Bruker AXS, 1997-2012). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT 8.x (Bruker AXS, 1997-2011)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            103429
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.029
_diffrn_reflns_theta_min         1.525
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             1969
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.504
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         13502
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0848P)^2^+5.8864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10336
_reflns_number_total             13502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03262d2.cif
_cod_data_source_block           co_hr8
_cod_depositor_comments
'Adding full bibliography for 7033230--7033235.cif.'
_cod_original_cell_volume        4233(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7033232
_audit_block_refno               1550
_audit_block_usercomment         HR515
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8 of O8, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H5 of O5
2. Restrained distances
 O81-C81 \\sim O81-C83A \\sim O81-C83B
 with sigma of 0.02
 C81-C82 \\sim C83A-C84A \\sim C83B-C84B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C37 \\sim C36 \\sim C81 \\sim C82 \\sim C83A \\sim C84A \\sim C83B \\sim C84B: within 1A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Same fragment restrains
{B1, F11, F12, F13, F14}
as
{B2, F21, F22, F23, F24}
5. Others
 Sof(O7)=1-FVAR(1)
 Sof(O5)=Sof(H5)=Sof(O6)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C83B)=Sof(H83C)=Sof(H83D)=Sof(C84B)=Sof(H84D)=Sof(H84E)=Sof(H84F)=1-FVAR(2)
 Sof(C83A)=Sof(H83A)=Sof(H83B)=Sof(C84A)=Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(2)
6.a Riding coordinates:
 O8(H8)
6.b Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C25(H25)
6.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C81(H81A,H81B), C83A(H83A,H83B), C83B(H83C,H83D)
6.d Me refined with riding coordinates:
 C84A(H84A,H84B,H84C), C84B(H84D,H84E,H84F)
6.e 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)
6.f Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C37(H37A,H37B,
 H37C), C36(H36A,H36B,H36C), C82(H82A,H82B,H82C)
6.g Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.896
_shelx_res_checksum              4817