Iron(ii) complexes of 2,6-di(1H-pyrazol-3-yl)-pyridine derivatives with hydrogen bonding and sterically bulky substituents.
Roberts, Thomas D.; Little, Marc A.; Kershaw Cook, Laurence J.; Halcrow, Malcolm A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 7577–7588; doi:10.1039/c4dt00355a

data_7029572
_publ_section_title
;
 Iron(ii) complexes of 2,6-di(1H-pyrazol-3-yl)-pyridine derivatives with
 hydrogen bonding and sterically bulky substituents.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7577
_journal_page_last               7588
_journal_paper_doi               10.1039/c4dt00355a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C32 H38 Fe N10, 2[B F4], 2.6[C4 H10 O], 0.25[C2 H3 F3 O]]'
_chemical_formula_sum            'C42.9 H64.75 B2 F8.75 Fe N10 O2.85'
_chemical_formula_weight         1009.92
_chemical_name_systematic
; 
Bis-[2-{5-methyl-1H-pyrazol-3-yl}-6-2-{5-tertbutyl-1H-pyrazol-3-yl}pyridine]-
iron(II) ditetrafluoroborate diethyl ether/2,2,2-trifluoroethanol 
solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1739(5)
_cell_length_b                   17.9832(6)
_cell_length_c                   19.9978(7)
_cell_measurement_reflns_used    58452
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      1.35
_cell_volume                     5435.2(3)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58452
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2119
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         13077
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1572P)^2^+5.3495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2349
_refine_ls_wR_factor_ref         0.2626
_reflns_number_gt                9242
_reflns_number_total             13077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00355a3.cif
_cod_data_source_block           tdr166lt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7029568--7029572.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C42.90 H64.75 B2 F8.75 Fe N10 O2.85'
_cod_database_code               7029572