Incorporation of Pyrazine and Bipyridine Linkers with High-Spin Fe(II) and Co(II) in a Metal-Organic Framework.
Kawamura, Airi; Greenwood, Arin R.; Filatov, Alexander S.; Gallagher, Audrey T.; Galli, Giulia; Anderson, John S.; Inorganic chemistry 56 (2017) 3349–3356; doi:10.1021/acs.inorgchem.6b02883

data_4345327
_publ_section_title
;
 Incorporation of Pyrazine and Bipyridine Linkers with High-Spin Fe(II)
 and Co(II) in a Metal-Organic Framework.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3349
_journal_page_last               3356
_journal_paper_doi               10.1021/acs.inorgchem.6b02883
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C12 H8 Fe N2 O4'
_chemical_formula_sum            'C12 H8 Fe N2 O4'
_chemical_formula_weight         300.05
_space_group_crystal_system      hexagonal
_space_group_IT_number           175
_space_group_name_Hall           '-P 6'
_space_group_name_H-M_alt        'P 6/m'
_symmetry_space_group_name_Hall  '-P 6'
_symmetry_space_group_name_H-M   'P 6/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.644(2)
_cell_length_b                   24.644(2)
_cell_length_c                   7.1068(6)
_cell_measurement_reflns_used    7030
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.52
_cell_volume                     3737.9(5)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23375
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.037
_diffrn_reflns_theta_max         25.037
_diffrn_reflns_theta_min         2.525
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1328 before and 0.0750 after correction.
The Ratio of minimum to maximum transmission is 0.5725.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.800
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.698
_refine_diff_density_min         -1.714
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0794P)^2^+7.6420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1929
_reflns_number_total             2407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02883_si_002.cif
_cod_data_source_block           full_sq
_cod_depositor_comments          'Adding full bibliography for 4345327.cif.'
_cod_original_cell_volume        3738.0(7)
_cod_database_code               4345327
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 O3, O4, C4, C5, C6, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10)
;
_shelx_res_checksum              8565
_shelx_hkl_checksum              76375
_shelx_fab_checksum              59042
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'