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_7701808
_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
'C72 H56 Fe4 N56, 8(B F4), 0.5(C3 H4 B F3 N2), 5.9(C2 H3 N1)'
_chemical_formula_sum            'C85.3 H75.7 B8.5 F33.5 Fe4 N62.9'
_chemical_formula_weight         2933.77
_chemical_name_systematic
;
Octakis[2,4-di(pyrazol-1-yl)-1,3,5-triazine]-tetrairon(II)
octa-tetrafluoroborate hemi[2-(trifluoroboryl)-1H-pyrazole]
acetonitrile (8/5.9) solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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
;
2019-10-07 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                97.839(2)
_cell_angle_beta                 91.234(3)
_cell_angle_gamma                105.400(3)
_cell_formula_units_Z            2
_cell_length_a                   16.1862(6)
_cell_length_b                   17.2352(5)
_cell_length_c                   23.7427(7)
_cell_measurement_reflns_used    20214
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.63
_cell_measurement_theta_min      3.50
_cell_volume                     6314.5(4)
_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 0.952
_diffrn_measured_fraction_theta_max 0.932
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54575
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.92
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.676
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.506
_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            orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1754
_refine_ls_number_reflns         23884
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0777
_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^)+(0.1416P)^2^+9.8485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2353
_reflns_number_gt                19787
_reflns_number_total             23884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           fe(bpt)2
_cod_original_formula_sum        'C85.30 H75.70 B8.50 F33.50 Fe4 N62.90'
_cod_database_code               7701808
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B143-F44A = B143-F45A = B143-F46A = B143-F47A
 1.39455 with sigma of 0.02
 B143-F44B = B143-F45B = B143-F46B = B143-F47B
 1.39455 with sigma of 0.02
 F44A-F45A = F44A-F46A = F44A-F47A = F45A-F46A = F45A-F47A = F46A-F47A
 2.2773 with sigma of 0.02
 F44B-F45B = F44B-F46B = F44B-F47B = F45B-F46B = F45B-F47B = F46B-F47B
 2.2773 with sigma of 0.02
 B48A-F49A = B48A-F50A = B48A-F51A = B48A-F52A
 1.39455 with sigma of 0.02
 B48B-F49B = B48B-F50B = B48B-F51B = B48B-F52B
 1.39455 with sigma of 0.02
 F49A-F50A = F49A-F51A = F49A-F52A = F50A-F51A = F50A-F52A = F51A-F52A
 2.2773 with sigma of 0.02
 F49B-F50B = F49B-F51B = F49B-F52B = F50B-F51B = F50B-F52B = F51B-F52B
 2.2773 with sigma of 0.02
 B58A-F59A = B58A-F60A = B58A-F61A = B58A-F62A
 1.39455 with sigma of 0.02
 B58B-F59B = B58B-F60B = B58B-F61B = B58B-F62B
 1.39455 with sigma of 0.02
 F59A-F60A = F59A-F61A = F59A-F62A = F60A-F61A = F60A-F62A = F61A-F62A
 2.2773 with sigma of 0.02
 F59B-F60B = F59B-F61B = F59B-F62B = F60B-F61B = F60B-F62B = F61B-F62B
 2.2773 with sigma of 0.02
 C203-C204 = C206-C207
 1.48 with sigma of 0.02
 C204-N205 = C207-N208
 1.15 with sigma of 0.02
 C203-N205 = C206-N208
 2.63 with sigma of 0.02
 C106-N12B = N12B-N13B = N13B-C14B = C14B-C15B = C15B-C16B = C16B-N12B
 1.38 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: N12A(0.67) N13A(0.67) C14A(0.67) H14A(0.67) C15A(0.67) H15A(0.67)
 C16A(0.67) H16A(0.67) N12B(0.33) N13B(0.33) C14B(0.33) H14B(0.33) C15B(0.33)
 H15B(0.33) C16B(0.33) H16B(0.33) F44A(0.5) F45A(0.5) F46A(0.5) F47A(0.5)
 F44B(0.5) F45B(0.5) F46B(0.5) F47B(0.5) B48A(0.5) F49A(0.5) F50A(0.5)
 F51A(0.5) F52A(0.5) B48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5) F52B(0.5)
 B58A(0.5) F59A(0.5) F60A(0.5) F61A(0.5) F62A(0.5) B58B(0.5) F59B(0.5)
 F60B(0.5) F61B(0.5) F62B(0.5) N173(0.5) N174(0.5) H174(0.5) C175(0.5)
 H175(0.5) C176(0.5) H176(0.5) C177(0.5) H177(0.5) B178(0.5) F179(0.5)
 F180(0.5) F181(0.5) C182(0.7) H18A(0.7) H18B(0.7) H18C(0.7) C183(0.7)
 N184(0.7) C185(0.8) H18D(0.8) H18E(0.8) H18F(0.8) C186(0.8) N187(0.8)
 C188(0.7) H18G(0.7) H18H(0.7) H18I(0.7) C189(0.7) N190(0.7) C194(0.9)
 H19D(0.9) H19E(0.9) H19F(0.9) C195(0.9) N196(0.9) C197(0.8) H19G(0.8)
 H19H(0.8) H19I(0.8) C198(0.8) N199(0.8) C200(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C201(0.5) N202(0.5) C203(0.3) H20D(0.3) H20E(0.3) H20F(0.3)
 C204(0.3) N205(0.3) C206(0.2) H20G(0.2) H20H(0.2) H20I(0.2) C207(0.2) N208(0.2)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C24(H24),
 C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C40(H40), C45(H45),
  C46(H46), C47(H47), C50(H50), C51(H51), C52(H52), C56(H56), C61(H61),
 C62(H62), C63(H63), C66(H66), C67(H67), C68(H68), C72(H72), C77(H77), C78(H78),
  C79(H79), C82(H82), C83(H83), C84(H84), C88(H88), C93(H93), C94(H94),
 C95(H95), C98(H98), C99(H99), C100(H100), C104(H104), C109(H109), C110(H110),
 C111(H111), C14A(H14A), C15A(H15A), C16A(H16A), C14B(H14B), C15B(H15B),
 C16B(H16B), C120(H120), C125(H125), C126(H126), C127(H127), C130(H130),
 C131(H131), C132(H132), N174(H174), C175(H175), C176(H176), C177(H177)
4.b Idealised Me refined as rotating group:
 C182(H18A,H18B,H18C), C185(H18D,H18E,H18F), C188(H18G,H18H,H18I), C191(H19A,
 H19B,H19C), C194(H19D,H19E,H19F), C197(H19G,H19H,H19I), C200(H20A,H20B,H20C),
 C203(H20D,H20E,H20F), C206(H20G,H20H,H20I)
;