Supramolecular aggregation of Ni(salen) with (C6F5)2Hg and [o-C6F4Hg]3.
Tsunoda, Mitsukimi; Fleischmann, Martin; Jones, J. Stuart; Bhuvanesh, Nattamai; Scheer, Manfred; Gabbaï, François P; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5045–5051; doi:10.1039/c5dt01887k

data_7038298
_publ_section_title
;
 Supramolecular aggregation of Ni(salen) with (C6F5)2Hg and [o-C6F4Hg]3.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5045
_journal_page_last               5051
_journal_paper_doi               10.1039/c5dt01887k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 F10 Hg, 1(C16 H14 N2 Ni O2)'
_chemical_formula_sum            'C28 H14 F10 Hg N2 Ni O2'
_chemical_formula_weight         859.71
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2016-01-17 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.806(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1203(7)
_cell_length_b                   24.870(2)
_cell_length_c                   14.1415(15)
_cell_measurement_reflns_used    6688
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      26.712
_cell_measurement_theta_min      2.885
_cell_volume                     2501.2(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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  0.0760
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21406
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.631
_diffrn_reflns_theta_min         1.638
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.992
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1157 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.6788.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_description       blade
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.147
_refine_diff_density_min         -3.094
_refine_diff_density_rms         0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         5756
_refine_ls_number_restraints     969
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0620P)^2^+40.0929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3811
_reflns_number_total             5756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01887k2.cif
_cod_data_source_block           hgni
_cod_depositor_comments
'Adding full bibliography for 7038296--7038298.cif.'
_cod_database_code               7038298
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.488
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Ni1S \\sim O1S \\sim O2S \\sim N1S \\sim N2S \\sim C1S \\sim C2S \\sim C3S
\\sim C4S \\sim C5S \\sim C6S \\sim C7S \\sim C8S \\sim C9S \\sim C10S \\sim
C11S \\sim C12S \\sim C13S \\sim C14S \\sim C15S \\sim C16S \\sim Ni1T \\sim
O1T \\sim O2T \\sim N1T \\sim N2T \\sim C1T \\sim C2T \\sim C3T \\sim C4T \\sim
C5T \\sim C6T \\sim C7T \\sim C8T \\sim C9T \\sim C10T \\sim C11T \\sim C12T
\\sim C13T \\sim C14T \\sim C15T \\sim C16T: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C16S) = Uanis(C1T)
Uanis(C7T) = Uanis(C10S)
Uanis(Ni1S) = Uanis(Ni1T)
Uanis(O2S) = Uanis(O2T)
Uanis(O1S) = Uanis(O1T)
Uanis(N1T) = Uanis(N1S)
Uanis(N2T) = Uanis(N2S)
3. Rigid body (RIGU) restrains
 Ni1S, O1S, O2S, N1S, N2S, C1S, C2S, C3S, C4S, C5S, C6S, C7S, C8S, C9S, C10S,
 C11S, C12S, C13S, C14S, C15S, C16S, Ni1T, O1T, O2T, N1T, N2T, C1T, C2T, C3T,
 C4T, C5T, C6T, C7T, C8T, C9T, C10T, C11T, C12T, C13T, C14T, C15T, C16T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Ni1S, O1S, O2S, N1S, N2S, C1S, C2S, C3S, C4S, C5S, C6S, C7S, C8S, C9S, C10S,
C11S, C12S, C13S, C14S, C15S, C16S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Ni1T, O1T, O2T, N1T, N2T, C1T, C2T, C3T, C4T, C5T, C6T, C7T, C8T, C9T, C10T,
C11T, C12T, C13T, C14T, C15T, C16T}
5. Others
 Sof(Ni1T)=Sof(O1T)=Sof(O2T)=Sof(N1T)=Sof(N2T)=Sof(C1T)=Sof(C2T)=Sof(H2T)=
 Sof(C3T)=Sof(H3T)=Sof(C4T)=Sof(H4T)=Sof(C5T)=Sof(H5T)=Sof(C6T)=Sof(C7T)=
 Sof(H7T)=Sof(C8T)=Sof(H8TA)=Sof(H8TB)=Sof(C9T)=Sof(H9TA)=Sof(H9TB)=Sof(C10T)=
 Sof(H10T)=Sof(C11T)=Sof(C12T)=Sof(H12T)=Sof(C13T)=Sof(H13T)=Sof(C14T)=
 Sof(H14T)=Sof(C15T)=Sof(H15T)=Sof(C16T)=1-FVAR(1)
 Sof(Ni1S)=Sof(O1S)=Sof(O2S)=Sof(N1S)=Sof(N2S)=Sof(C1S)=Sof(C2S)=Sof(H2S)=
 Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(C7S)=
 Sof(H7S)=Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(C10S)=
 Sof(H10S)=Sof(C11S)=Sof(C12S)=Sof(H12S)=Sof(C13S)=Sof(H13S)=Sof(C14S)=
 Sof(H14S)=Sof(C15S)=Sof(H15S)=Sof(C16S)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8S(H8SA,H8SB), C9S(H9SA,H9SB), C8T(H8TA,H8TB), C9T(H9TA,H9TB)
6.b Aromatic/amide H refined with riding coordinates:
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C7S(H7S), C10S(H10S), C12S(H12S),
 C13S(H13S), C14S(H14S), C15S(H15S), C2T(H2T), C3T(H3T), C4T(H4T), C5T(H5T),
 C7T(H7T), C10T(H10T), C12T(H12T), C13T(H13T), C14T(H14T), C15T(H15T)
;
_shelx_res_checksum              9942
_olex2_submission_special_instructions 'No special instructions were received'