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_7702208
_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         'C66 H68 Cl4 N6 O Zn2, 6(C2 H3 N)'
_chemical_formula_sum            'C78 H86 Cl4 N12 O Zn2'
_chemical_formula_weight         1480.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-18 deposited with the CCDC.
2018-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.956(6)
_cell_length_b                   19.724(5)
_cell_length_c                   23.052(5)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.40
_cell_volume                     7710(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53294
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         1.201
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 2172 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9399
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0961
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+113.1926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2428
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                6210
_reflns_number_total             9399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02347f2.cif
_cod_data_source_block           compound11-zncl2
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7702208
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(4)
 0.10(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N1S_2, C1S_2, C2S_2}
{N1S_3, C1S_3, C2S_3}
{N1S_4, C1S_4, C2S_4}
as
{N1S_1, C1S_1, C2S_1} sigma for 1-2: 0.005 1-3: 0.005
6. Others
 Fixed Sof: N1S(0.5) C1S(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5) N1S(0.5)
 C1S(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C12A(H12A), C23A(H23A), C21A(H21A), C4A(H4A), C6A(H6A), C6(H6),
 C5(H5), C4(H4), C2(H2)
7.b Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C17A(H17A,H17B,H17C), C16A(H16A,H16B,H16C), C25A(H25A,
 H25B,H25C), C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C), C1A(H1AA,H1AB,H1AC),
 C9A(H9AA,H9AB,H9AC), C2S(H2SA,H2SB,H2SC), C2S(H2SA,H2SB,H2SC), C2S(H2SA,H2SB,
 H2SC), C2S(H2SA,H2SB,H2SC)
;
_olex2_submission_special_instructions 'No special instructions were received'