#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:23:56 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180260 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/46/7114654.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7114654
loop_
_publ_author_name
'Jonathan J. Loughrey'
'Tim P. Comyn'
'David C. Apperley'
'Marc A. Little'
'Malcolm A. Halcrow'
_publ_section_title
;
 Complex thermal expansion properties in a molecular honeycomb lattice
;
_journal_name_full               Chem.Commun.
_journal_page_first              7601
_journal_paper_doi               10.1039/C4CC02198C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C21 H18 Fe N12, 2[B F4], 3[H2 O]'
_chemical_formula_sum            'C21 H24 B2 F8 Fe N12 O3'
_chemical_formula_weight         721.99
_chemical_name_systematic
; 
Tris[pyrazol-3-ylpyrazine]iron(II) ditetrafluoroborate trihydrate 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.6729(5)
_cell_length_b                   12.6729(5)
_cell_length_c                   10.9338(6)
_cell_measurement_reflns_used    11971
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.63
_cell_volume                     1520.74(12)
_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      300(2)
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11971
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.846
_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            brown
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2366
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0383
_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/[σ²(Fo²)+(0.0769P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                2218
_reflns_number_total             2366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02198c2.cif
_cod_data_source_block           rs1n300a
_cod_original_sg_symbol_H-M      'P 31c'
_cod_database_code               7114654
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.6667 0.3333 0.32787(4) 0.02863(14) Uani 1 3 d S . .
N2 N 0.55412(18) 0.3678(2) 0.42350(16) 0.0345(4) Uani 1 1 d . . .
C3 C 0.4834(3) 0.3053(3) 0.5190(2) 0.0466(6) Uani 1 1 d . . .
H3 H 0.4856 0.2376 0.5486 0.056 Uiso 1 1 calc R . .
C4 C 0.4073(3) 0.3406(3) 0.5737(3) 0.0575(8) Uani 1 1 d . . .
H4 H 0.3601 0.2959 0.6399 0.069 Uiso 1 1 calc R . .
N5 N 0.3990(2) 0.4355(3) 0.5355(2) 0.0549(6) Uani 1 1 d . . .
C6 C 0.4676(3) 0.4970(3) 0.4417(3) 0.0484(6) Uani 1 1 d . . .
H6 H 0.4636 0.5639 0.4127 0.058 Uiso 1 1 calc R . .
C7 C 0.5458(2) 0.4652(2) 0.3846(2) 0.0371(5) Uani 1 1 d . . .
C8 C 0.6233(2) 0.5282(2) 0.2815(2) 0.0379(5) Uani 1 1 d . . .
N9 N 0.68321(18) 0.4744(2) 0.23615(18) 0.0333(4) Uani 1 1 d . . .
N10 N 0.75454(19) 0.54807(19) 0.14688(19) 0.0418(4) Uani 1 1 d . . .
H10 H 0.8027 0.5344 0.1030 0.050 Uiso 1 1 calc R . .
C11 C 0.7410(3) 0.6454(3) 0.1350(3) 0.0590(8) Uani 1 1 d . . .
H11 H 0.7813 0.7083 0.0790 0.071 Uiso 1 1 calc R . .
C12 C 0.6575(3) 0.6367(3) 0.2198(3) 0.0557(8) Uani 1 1 d . . .
H12 H 0.6297 0.6912 0.2332 0.067 Uiso 1 1 calc R . .
B13 B 0.6667 0.3333 0.8196(9) 0.0549(13) Uani 1 3 d S . .
F14 F 0.6667 0.3333 0.9453(4) 0.0770(11) Uani 1 3 d S . .
F15 F 0.7172(3) 0.4516(2) 0.7829(3) 0.1045(9) Uani 1 1 d . . .
B16A B 0.149(2) 0.159(2) 0.858(2) 0.053(8) Uiso 0.10 1 d PD A 1
F17A F 0.2255(16) 0.2763(17) 0.8216(17) 0.061(4) Uiso 0.10 1 d PD A 1
F18A F 0.118(4) 0.090(3) 0.758(3) 0.158(16) Uiso 0.10 1 d PD A 1
F19A F 0.205(4) 0.121(3) 0.933(3) 0.161(17) Uiso 0.10 1 d PD A 1
F20A F 0.053(3) 0.154(3) 0.913(3) 0.154(16) Uiso 0.10 1 d PD A 1
B16B B 0.124(2) 0.157(2) 0.882(2) 0.049(8) Uiso 0.09 1 d PD B 2
F17B F 0.217(3) 0.223(3) 0.807(3) 0.119(12) Uiso 0.09 1 d PD B 2
F18B F 0.029(3) 0.075(2) 0.816(2) 0.090(7) Uiso 0.09 1 d PD . 2
F19B F 0.151(3) 0.095(3) 0.961(3) 0.111(11) Uiso 0.09 1 d PD B 2
F20B F 0.089(2) 0.227(2) 0.938(2) 0.082(7) Uiso 0.09 1 d PD B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N9 Fe1 N9 96.33(8) 2_655 .
N9 Fe1 N2 174.09(10) . 2_655
N9 Fe1 N2 88.87(9) 2_655 .
N9 Fe1 N2 80.25(8) . .
N2 Fe1 N2 94.80(7) 2_655 .
C3 N2 C7 116.5(2) . .
C3 N2 Fe1 128.31(19) . .
C7 N2 Fe1 115.19(15) . .
N2 C3 C4 120.7(3) . .
N5 C4 C3 122.7(2) . .
C6 N5 C4 116.9(2) . .
N5 C6 C7 122.2(3) . .
N2 C7 C6 120.9(2) . .
N2 C7 C8 114.00(19) . .
C6 C7 C8 125.1(2) . .
N9 C8 C12 110.3(2) . .
N9 C8 C7 114.0(2) . .
C12 C8 C7 135.6(2) . .
N10 N9 C8 105.7(2) . .
N10 N9 Fe1 137.08(16) . .
C8 N9 Fe1 116.27(15) . .
C11 N10 N9 111.2(2) . .
N10 C11 C12 108.2(2) . .
C11 C12 C8 104.7(2) . .
F15 B13 F15 111.7(4) 2_655 .
F15 B13 F14 107.1(4) . .
F18A B16A F20A 111.9(18) . .
F18A B16A F19A 107.7(17) . .
F20A B16A F19A 110.3(17) . .
F18A B16A F17A 107.0(17) . .
F20A B16A F17A 108.7(16) . .
F19A B16A F17A 111.1(17) . .
F20B B16B F19B 111.3(17) . .
F20B B16B F17B 111.2(17) . .
F19B B16B F17B 111.1(17) . .
F20B B16B F18B 107.0(16) . .
F19B B16B F18B 107.3(17) . .
F17B B16B F18B 108.9(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N9 1.967(2) .
Fe1 N2 1.985(2) .
N2 C3 1.346(3) .
N2 C7 1.359(3) .
C3 C4 1.385(4) .
C4 N5 1.326(4) .
N5 C6 1.319(3) .
C6 C7 1.390(3) .
C7 C8 1.445(3) .
C8 N9 1.344(3) .
C8 C12 1.392(4) .
N9 N10 1.341(3) .
N10 C11 1.334(4) .
C11 C12 1.370(4) .
B13 F15 1.363(4) .
B13 F14 1.374(10) .
B16A F18A 1.33(2) .
B16A F20A 1.33(2) .
B16A F19A 1.33(2) .
B16A F17A 1.36(2) .
B16B F20B 1.32(2) .
B16B F19B 1.33(2) .
B16B F17B 1.34(2) .
B16B F18B 1.34(2) .
F18B F18B 1.45(4) 2
F18B F18B 1.45(4) 3
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 N5 0.86 2.02 2.826(3) 156.7 5_664
C4 H4 F17A 0.93 2.55 3.383(19) 149.5 .
C4 H4 F17B 0.93 2.40 3.30(3) 163.1 .
