Molecular Squares, Coordination Polymers and Mononuclear Complexes Supported by 2,4-Dipyrazolyl-6H-1,3,5-triazine and 4,6-Dipyrazolylpyrimidine Ligands
Capel Berdiell, Izar; Farmiloe, Sarah E.; Kulmaczewski, Rafal; Halcrow, Malcolm; Dalton Transactions  (2019) –; doi:10.1039/C9DT04003J

data_7701828
_publ_section_title
;
 Molecular Squares, Coordination Polymers and Mononuclear Complexes
 Supported by 2,4-Dipyrazolyl-6H-1,3,5-triazine and
 4,6-Dipyrazolylpyrimidine Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04003J
_journal_year                    2019
_chemical_formula_moiety         'C22 H16 Fe N14 Se2, 0.5(C3 H6 O)'
_chemical_formula_sum            'C23.5 H19 Fe N14 O0.5 Se2'
_chemical_formula_weight         719.30
_chemical_name_systematic
'Bis-[4,6-di(pyrazol-1-yl)pyrimidine]-di[isoselenocyanato]iron(II)hemi-acetone solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.447(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7269(5)
_cell_length_b                   14.6440(6)
_cell_length_c                   16.1908(7)
_cell_measurement_reflns_used    3443
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.32
_cell_measurement_theta_min      3.84
_cell_volume                     2845.4(2)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10897
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.54
_diffrn_reflns_theta_min         3.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.549
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5537
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0636P)^2^+2.4629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                4193
_reflns_number_total             5537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           150seac
_cod_original_formula_sum        'C23.50 H19 Fe N14 O0.50 Se2'
_cod_database_code               7701828
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O40A-C41A = O40B-C41B
 1.22 with sigma of 0.02
 C41A-C42A = C41A-C43A = C41B-C42B = C41B-C43B
 1.51 with sigma of 0.02
 C42A-C43A = C42B-C43B
 2.62 with sigma of 0.02
 O40A-C42A = O40A-C43A = O40B-C42B = O40B-C43B
 2.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O40A \\sim C41A \\sim C42A \\sim C43A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
O40B \\sim C41B \\sim C42B \\sim C43B: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Se7A(0.57) Se7B(0.43) O40A(0.25) C41A(0.25) C42A(0.25) H42A(0.25)
 H42B(0.25) H42C(0.25) C43A(0.25) H43A(0.25) H43B(0.25) H43C(0.25) O40B(0.25)
 C41B(0.25) C42B(0.25) H42D(0.25) H42E(0.25) H42F(0.25) C43B(0.25) H43D(0.25)
 H43E(0.25) H43F(0.25)
5.a Me refined with riding coordinates:
 C42A(H42A,H42B,H42C), C43A(H43A,H43B,H43C), C42B(H42D,H42E,H42F), C43B(H43D,
 H43E,H43F)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C24(H24), C27(H27), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
;