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_7702207
_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         'C78 H91 Cl4 N6 Ni2, 7(C4 H8 O)'
_chemical_formula_sum            'C106 H147 Cl4 N6 Ni2 O7'
_chemical_formula_weight         1876.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-18
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.524(6)
_cell_length_b                   23.041(8)
_cell_length_c                   24.556(8)
_cell_measurement_reflns_used    9716
_cell_measurement_temperature    100.1(1)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.27
_cell_volume                     9915(6)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.10(10)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.932
_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  0.0628
_diffrn_reflns_av_unetI/netI     0.1110
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59940
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.143
_diffrn_reflns_theta_min         1.212
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1283 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.8567.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       plate
_exptl_crystal_F_000             4020
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 5647 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         24266
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                16363
_reflns_number_total             24266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02347f2.cif
_cod_data_source_block           9_
_cod_database_code               7702207
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.899
_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. Restrained distances
 O1S-C1S = O1S-C4S
 1.4 with sigma of 0.02
 H16H-H36C
 2 with sigma of 0.02
 C2G-C14 = C15-C14
 1.4 with sigma of 0.02
 C2G-C15
 2.346 with sigma of 0.04
 C13-C14
 2.34 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) = Uanis(C4S)
Uanis(C2G) = Uanis(C15)
Uanis(C31B) = Uanis(C32B) = Uanis(C33B) = Uanis(C34B) = Uanis(C35B) =
Uanis(C36B)
4. Others
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C34B)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=Sof(C36B)=Sof(H36A)=Sof(H36B)=Sof(H36C)=1-FVAR(1)
 Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C33B)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C35B)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Fixed U11: C1(0.02051)
 Fixed U12: C1(-0.00236)
 Fixed U13: C1(-0.00002)
 Fixed U22: C1(0.02117)
 Fixed U23: C1(0.00132)
 Fixed U33: C1(0.01536)
5.a Secondary CH2 refined with riding coordinates:
 C26A(H26A,H26B), C1S(H1SA,H1SB), C2AA(H2AA,H2AB), C2G(H2GA,H2GB), C2S(H2SA,
 H2SB), C3AA(H3AA,H3AB), C3S(H3SA,H3SB), C4AA(H4AA,H4AB), C4S(H4SA,H4SB),
 C5S(H5SA,H5SB), C6S(H6SA,H6SB), C8S(H8SA,H8SB), C9S(H9SA,H9SB), C10S(H10A,
 H10B), C11S(H11A,H11B), C12S(H12C,H12D), C13(H13A,H13B), C13S(H13C,H13D),
 C14(H14C,H14D), C14S(H14E,H14F), C15(H15A,H15B), C15S(H15C,H15D), C16S(H16G,
 H16H), C17S(H17G,H17H), C19S(H19G,H19H), C20S(H20G,H20H), C25S(H25A,H25B),
 C26S(H26D,H26E), C27S(H27A,H27B)
5.b Me refined with riding coordinates:
 C1B(H1BA,H1BB,H1BC)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C4A(H4A), C4B(H4B), C6A(H6A), C6B(H6B), C7(H7),
 C8(H8), C9(H9), C12A(H12A), C12B(H12B), C14A(H14A), C14B(H14B), C24A(H24A),
 C24B(H24B), C26B(H26C)
5.d Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C16A(H16A,H16B,
 H16C), C16B(H16D,H16E,H16F), C17A(H17A,H17B,H17C), C17B(H17D,H17E,H17F),
 C19A(H19A,H19B,H19C), C19B(H19D,H19E,H19F), C20A(H20A,H20B,H20C), C20B(H20D,
 H20E,H20F), C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C28A(H28A,H28B,H28C),
 C28B(H28D,H28E,H28F), C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C31A(H31A,
 H31B,H31C), C31B(H31D,H31E,H31F), C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F),
 C33A(H33A,H33B,H33C), C33B(H33D,H33E,H33F), C34B(H34A,H34B,H34C), C35B(H35A,
 H35B,H35C), C36B(H36A,H36B,H36C)
;
_shelx_res_checksum              85941
_olex2_submission_special_instructions 'No special instructions were received'