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_7702206
_publ_section_title
;
 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         'C33 H42 B N3 O2'
_chemical_formula_sum            'C33 H42 B N3 O2'
_chemical_formula_weight         523.51
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-07-18 deposited with the CCDC.
2018-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5588(4)
_cell_length_b                   10.1750(3)
_cell_length_c                   26.5199(9)
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.67
_cell_volume                     3117.23(18)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35120
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1482 before and 0.0644 after correction. The Ratio of minimum to maximum transmission is 0.7952. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6107
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1190P)^2^+1.2943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2306
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                4527
_reflns_number_total             6107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02347f2.cif
_cod_data_source_block           5
_cod_database_code               7702206
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C1 \\sim O2-C2 \\sim O1-C21 \\sim O2-C22
 with sigma of 0.005
 C1-C2 \\sim C21-C22
 with sigma of 0.005
 C1-C3 \\sim C1-C4 \\sim C2-C5 \\sim C2-C6 \\sim C21-C23 \\sim C21-C24 \\sim
C22-C25 \\sim C22-C26
 with sigma of 0.005
3. Others
 Sof(C21)=Sof(C22)=Sof(C23)=Sof(H23B)=Sof(H23C)=Sof(H23D)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4B)=Sof(H4C)=
 Sof(H4D)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6B)=Sof(H6C)=Sof(H6D)=
 FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C12A(H12A), C14A(H14A), C21A(H21A), C23A(H23A)
4.b Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C9A(H9AA,H9AB,H9AC), C16A(H16A,H16B,H16C), C17A(H17A,
 H17B,H17C), C18A(H18A,H18B,H18C), C25A(H25A,H25B,H25C), C26A(H26A,H26B,H26C),
 C27A(H27A,H27B,H27C), C3(H3A,H3B,H3C), C4(H4B,H4C,H4D), C5(H5A,H5B,H5C),
 C6(H6B,H6C,H6D), C23(H23B,H23C,H23D), C24(H24A,H24B,H24C), C25(H25D,H25E,H25F),
  C26(H26D,H26E,H26F)
;
_olex2_submission_special_instructions 'No special instructions were received'