Systematic study of the synthesis and coordination of 2-(1,2,3-triazol-4-yl)-pyridine to Fe(ii), Ni(ii) and Zn(ii); ion-induced folding into helicates, mesocates and larger architectures, and application to magnetism and self-selection.
Wu, Nan; Melan, Caroline F. C.; Stevenson, Kristina A.; Fleischel, Olivier; Guo, Huan; Habib, Fatemah; Holmberg, Rebecca J.; Murugesu, Muralee; Mosey, Nicholas J.; Nierengarten, Hélène; Petitjean, Anne; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14991–15005; doi:10.1039/c5dt00233h

data_7036017
_publ_section_title
;
 Systematic study of the synthesis and coordination of
 2-(1,2,3-triazol-4-yl)-pyridine to Fe(ii), Ni(ii) and Zn(ii); ion-induced
 folding into helicates, mesocates and larger architectures, and
 application to magnetism and self-selection.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14991
_journal_page_last               15005
_journal_paper_doi               10.1039/c5dt00233h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C51 H48 Fe2 N24, 4(B F4), 3(C2 H3 N), H2 O'
_chemical_formula_sum            'C57 H59 B4 F16 Fe2 N27 O'
_chemical_formula_weight         1597.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-2014 template'
_audit_update_record
;
2015-04-03 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                109.535(2)
_cell_angle_beta                 101.234(3)
_cell_angle_gamma                103.518(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8603(5)
_cell_length_b                   17.9020(7)
_cell_length_c                   17.9413(7)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.23
_cell_volume                     3894.0(3)
_computing_cell_refinement
' Saint V8.30A and SADABS V2012/1 (Apex2, v2013.10-0; Bruker AXS)'
_computing_data_collection
' APEX2 software package v2013.10-0 (Bruker AXS)'
_computing_data_reduction
' Saint V8.30A and SADABS V2012/1 (Apex2, v2013.10-0; Bruker AXS'
_computing_molecular_graphics    ' XP (SHELXTL-NT v6.14, Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    ' 'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart Apex2 CCD (Bruker AXS)'
_diffrn_measurement_method       'CCD rotation images, \w scans'
_diffrn_radiation_monochromator  'horizontal mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55597
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.275
_diffrn_source                   'Bruker AXS K780, fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Apex2, Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6855
_platon_squeeze_details
;Approximately 14% of the unit cell (560.2 \%a^3^) comprises a 
 region of disordered solvent molecules and their atoms could not
 be modeled as discrete atomic sites. Attempts to refine the peaks
 of the residual electron density as 0.5 Et2O and two molecules
 of MeCN within the asymmetric unit were unsuccessful. The
 program PLATON/SQUEEZE was used to calculate the contribution
 from the solvent region to the diffraction. The data were 
 corrected for the disordered electron density using the SQUEEZE
 routine as implemented in PLATON leading to set of solvent-free
 diffraction intensities. A total electron count of 127 electrons
 was found in the total solvent accessible void volume within the 
 unit cell.
 Expected molar volume/electron count for Et2O: 104.8 \%a^3^/42 e^-^.
 Expected molar volume/electron count for MeCN: 82 \%a^3^/22 e^-^.
 With this in mind, this accounts for additional four molecules
 of MeCN plus two 0.5(Et2O) within the unit cell and two molecules
 of MeCN plus one 0.5(Et2O) within the asymmetric unit (total
 electron count of 130 electrons within the unit cell). This 
 result is supported by the observations in the electron difference
 map.
 The modified data improved the R-factors (before SQUEEZE: 
 <i>R</i>~1~ = 0.0933, <i>wR</i>~2~ = 0.2561; largest peak and
 hole, 2.248 and -0.832 ^-^/A\%a^3^; after SQUEEZE: 
 <i>R</i>~1~ = 0.0588, <i>wR</i>~2~ = 0.1641; largest peak
 and hole, 1.429 and -0.778 ^-^/A\%a^3^). Derived values (formula
 weight, density, absorption coefficient) do not contain the 
 contribution of the disordered solvent.
;
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         15859
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+5.9446P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12812
_reflns_number_total             15859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00233h2.cif
_cod_data_source_block           ap28_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7036017.cif.
;
_cod_database_code               7036017
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.955
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2012-9
_shelx_res_checksum              69753
_shelx_fab_checksum              71546