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_7033235
_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
'2(C34 H36 Cl Mn N6 O6), Cl4 Mn, C H4 O'
_chemical_formula_sum            'C69 H76 Cl6 Mn3 N12 O13'
_chemical_formula_weight         1658.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.361(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.546(2)
_cell_length_b                   15.8473(17)
_cell_length_c                   23.647(2)
_cell_measurement_temperature    200(2)
_cell_volume                     7458.8(13)
_computing_cell_refinement       'CELL (STOE) & Cie. GmbH'
_computing_data_collection       'EXPOSE (STOE & Cie. GmbH)'
_computing_data_reduction        'INTEGRATE (STOE) & Cie. GmbH'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       'image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_unetI/netI     0.1142
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            88584
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.528
_diffrn_reflns_theta_min         2.601
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'STOE IPDS'
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             3420
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.511
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         22313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0608P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11153
_reflns_number_total             22313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03262d2.cif
_cod_data_source_block           hru13_sq
_cod_depositor_comments
;
Adding full bibliography for 7033230--7033235.cif.

2018-01-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         829.47
_cod_original_formula_moiety
'C34 H36 Cl Mn N6 O6, 0.5(Cl4 Mn), 0.5(C H4 O)'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_original_formula_sum        'C34.50 H38 Cl3 Mn1.50 N6 O6.50'
_cod_database_code               7033235
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.665
_shelxl_version_number           2014/6
_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.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C25(H25), C52(H52), C54(H54), C75(H75)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C56(H56A,H56B), C58(H58A,H58B)
2.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), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71),
 C72(H72), C73(H73), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83),
  C84(H84), C85(H85)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C36(H36A,H36B,
 H36C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C74(H74A,H74B,H74C), C86(H86A,
 H86B,H86C), C91(H91A,H91B,H91C)
2.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O55(H55), O91(H91)
;
_shelx_res_checksum              59909