Dinuclear tethered pyridine, diimine complexes.
Dammann, Wiebke; Buban, Tabea; Schiller, Carl; Burger, Peter; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12105–12117; doi:10.1039/c8dt02347f

data_7702210
_publ_section_title
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 Dinuclear tethered pyridine, diimine complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12105
_journal_page_last               12117
_journal_paper_doi               10.1039/c8dt02347f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H50 N6'
_chemical_formula_sum            'C40 H50 N6'
_chemical_formula_weight         614.86
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-18 deposited with the CCDC.
2018-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4198(2)
_cell_length_b                   11.24410(10)
_cell_length_c                   25.6150(3)
_cell_measurement_reflns_used    35329
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3870
_cell_measurement_theta_min      4.2850
_cell_volume                     3497.81(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            70576
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.508
_diffrn_reflns_theta_min         3.529
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.037
_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     465
_refine_ls_number_reflns         7316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0556P)^2^+0.8298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6627
_reflns_number_total             7316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02347f2.cif
_cod_data_source_block           compound_12
_cod_database_code               7702210
_shelx_shelxl_version_number     2014/7
_diffrn_standard_number          0
_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 C(H,H,H,H,H,H) groups
2. Others
 Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C15B)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=
 Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(2)
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=
 Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(2)
 Fixed Sof: H1CA(0.5) H1CB(0.5) H1CC(0.5) H1CD(0.5) H1CE(0.5) H1CF(0.5)
 H9BA(0.5) H9BB(0.5) H9BC(0.5) H9BD(0.5) H9BE(0.5) H9BF(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10A(H10A,H10B), C10B(H10C,H10D), C11A(H11A,H11B), C11B(H11C,H11D), C13A(H13A,
 H13B), C13B(H13C,H13D), C14A(H14A,H14B), C14B(H14C,H14D), C16A(H16A,H16B),
 C16B(H16C,H16D), C17A(H17A,H17B), C17B(H17C,H17D)
3.b Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C9A(H9AA,H9AB,H9AC), C12B(H12D,H12E,H12F), C18A(H18A,
 H18B,H18C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C4A(H4A), C4B(H4B), C5(H5), C6(H6), C6A(H6A),
 C6B(H6B), C7(H7)
3.d Disordered Me refined with riding coordinates:
 C1C(H1CA,H1CB,H1CC,H1CD,H1CE,H1CF)
3.e Disordered Me refined as rotating group:
 C9B(H9BA,H9BB,H9BC,H9BD,H9BE,H9BF)
3.f Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C18B(H18D,
 H18E,H18F)
;
_olex2_submission_special_instructions 'No special instructions were received'