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_7702212
_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
'C72 H68 F12 N6 O12 S4 Zn2, 0.5(C H2 Cl2), C4 H10 O'
_chemical_formula_sum            'C76.5 H78 Cl F12.5 N6 O12.5 S4 Zn2'
_chemical_formula_weight         1813.37
_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
_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                 103.5470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.401(3)
_cell_length_b                   16.5325(15)
_cell_length_c                   36.065(3)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.31
_cell_volume                     17622(3)
_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      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            263207
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.162
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       bar
_exptl_crystal_F_000             7460
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.106
_refine_diff_density_max         3.579
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2130
_refine_ls_number_reflns         40263
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0856
_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^)+(0.0596P)^2^+92.9299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29802
_reflns_number_total             40263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02347f2.cif
_cod_data_source_block           compound10-znotf2
_cod_original_formula_sum        'C76.50 H78 Cl F12.50 N6 O12.50 S4 Zn2'
_cod_database_code               7702212
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.760
_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
2. Uiso/Uaniso restraints and constraints
O01S_10 \\sim C01S_10 \\sim C02S_10 \\sim C03S_10 \\sim C04S_10: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C33) = Uanis(C26)
Uanis(C32) = Uanis(C25)
Uanis(C31) = Uanis(C24)
Uanis(C30) = Uanis(C23)
Uanis(C29) = Uanis(C22)
Uanis(C28) = Uanis(C21)
Uanis(F6A) = Uanis(F9A)
Uanis(F8A) = Uanis(F5A)
Uanis(F7A) = Uanis(F4A)
Uanis(C30A) = Uanis(C29A)
3. Rigid body (RIGU) restrains
 O01S_10, C01S_10, C02S_10, C03S_10, C04S_10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
5. Others
 Sof(F4A)=Sof(F5A)=Sof(F9A)=1-FVAR(1)
 Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(1)
 Sof(C29A)=1-FVAR(2)
 Sof(C30A)=FVAR(2)
 Sof(H20A)=Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=
 Sof(C25)=Sof(C26)=Sof(H27A)=1-FVAR(3)
 Sof(H20)=Sof(H27)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=
 Sof(H31)=Sof(C32)=Sof(C33)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C5S(H5SA,H5SB), C02S(H02A,H02B), C03S(H03A,H03B), C02S(H02A,H02B), C03S(H03A,
 H03B)
6.b Me refined with riding coordinates:
 C17A(H17A,H17B,H17C)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C20(H20), C20(H20A), C22(H22), C23(H23),
 C24(H24), C27(H27), C27(H27A), C29(H29), C30(H30), C31(H31), C34A(H34A),
 C34B(H34B), C36A(H36A), C36B(H36B), C42A(H42A), C42B(H42B), C44A(H44A),
 C44B(H44B), C51A(H51A), C51B(H51B), C53A(H53A), C53B(H53B), C2(H2), C3(H3),
 C4(H4), C4A(H4A), C4B(H4B), C6(H6), C6A(H6A), C6B(H6B), C8(H8), C9(H9),
 C10(H10), C12A(H12A), C12B(H12B), C13(H13), C14A(H14A), C14B(H14B), C21A(H21A),
  C21B(H21B), C23A(H23A), C23B(H23B)
6.d Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C39A(H39A,H39B,H39C), C39B(H39D,
 H39E,H39F), C46A(H46A,H46B,H46C), C46B(H46D,H46E,H46F), C47A(H47A,H47B,H47C),
 C47B(H47D,H47E,H47F), C48A(H48A,H48B,H48C), C48B(H48D,H48E,H48F), C55A(H55A,
 H55B,H55C), C55B(H55D,H55E,H55F), C56A(H56A,H56B,H56C), C56B(H56D,H56E,H56F),
 C57A(H57A,H57B,H57C), C57B(H57D,H57E,H57F), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,
 H1BC), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C16A(H16A,H16B,H16C),
 C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,
 H18E,H18F), C25A(H25A,H25B,H25C), C25B(H25D,H25E,H25F), C26A(H26A,H26B,H26C),
 C26B(H26D,H26E,H26F), C27A(H27B,H27C,H27D), C27B(H27E,H27F,H27G), C01S(H01A,
 H01B,H01C), C04S(H04A,H04B,H04C), C01S(H01A,H01B,H01C), C04S(H04A,H04B,H04C)
;
_olex2_submission_special_instructions 'No special instructions were received'