#------------------------------------------------------------------------------
#$Date: 2017-01-04 05:58:09 +0200 (Wed, 04 Jan 2017) $
#$Revision: 189786 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/92/7119259.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_7119259
loop_
_publ_author_name
'Darawsheh, M. D.'
'Barrios, L. A.'
'Roubeau, O.'
'Teat, S. J.'
'Aromí, G'
_publ_section_title
;
 Guest-tuned spin crossover in flexible supramolecular assemblies
 templated by a halide (Cl(-), Br(-) or I(-)).
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              569
_journal_page_last               572
_journal_paper_doi               10.1039/c6cc08906b
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
'2(C66 H48 Fe N18), 2(F6 P), Br, (H2 O), (H O)'
_chemical_formula_sum            'C132 H99 Br F12 Fe2 N36 O2 P2'
_chemical_formula_weight         2703.02
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-10-28 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.5619(5)
_cell_length_b                   13.5619(5)
_cell_length_c                   37.307(2)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.12
_cell_measurement_theta_min      2.24
_cell_volume                     5942.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            86965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        31.100
_diffrn_reflns_theta_max         31.183
_diffrn_reflns_theta_min         2.234
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       plate
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4960
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0630P)²+14.9133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4203
_reflns_number_total             4960
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc08906b2.cif
_cod_data_source_block           md422k_a
_cod_original_cell_volume        5942.4(5)
_cod_database_code               7119259
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br1 Br 1.0000 1.0000 0.7500 0.0435(3) Uani 1 6 d S T P
Fe1 Fe 1.0000 1.0000 0.90262(2) 0.01799(17) Uani 1 3 d S T P
N1 N 0.8673(2) 0.9820(2) 0.93089(6) 0.0211(5) Uani 1 1 d . . .
N2 N 0.8770(2) 0.87646(19) 0.87596(6) 0.0184(5) Uani 1 1 d . . .
N3 N 0.8670(2) 0.81287(19) 0.84711(6) 0.0192(5) Uani 1 1 d . . .
H3 H 0.9241 0.8231 0.8333 0.029 Uiso 1 1 calc R U .
N4 N 0.9043(2) 0.7340(2) 0.71294(6) 0.0218(5) Uani 1 1 d . . .
H4 H 0.9160 0.7932 0.7259 0.033 Uiso 1 1 calc R U .
N5 N 0.9629(2) 0.7407(2) 0.68298(6) 0.0230(5) Uani 1 1 d . . .
N6 N 0.9002(3) 0.5097(3) 0.62207(7) 0.0368(7) Uani 1 1 d . . .
C1 C 0.8686(3) 1.0476(3) 0.95809(7) 0.0242(6) Uani 1 1 d . . .
H1A H 0.9395 1.1101 0.9654 0.029 Uiso 1 1 calc R U .
C2 C 0.7710(3) 1.0277(3) 0.97591(8) 0.0283(6) Uani 1 1 d . . .
H2A H 0.7752 1.0774 0.9945 0.034 Uiso 1 1 calc R U .
C3 C 0.6672(3) 0.9353(3) 0.96650(8) 0.0292(6) Uani 1 1 d . . .
H3A H 0.5998 0.9188 0.9791 0.035 Uiso 1 1 calc R U .
C4 C 0.6640(3) 0.8672(3) 0.93825(8) 0.0250(6) Uani 1 1 d . . .
H4A H 0.5942 0.8028 0.9312 0.030 Uiso 1 1 calc R U .
C5 C 0.7644(2) 0.8946(2) 0.92057(7) 0.0204(5) Uani 1 1 d . . .
C6 C 0.7718(2) 0.8347(2) 0.88940(7) 0.0196(5) Uani 1 1 d . . .
C7 C 0.6930(2) 0.7427(2) 0.86875(7) 0.0215(5) Uani 1 1 d . . .
H7A H 0.6130 0.6982 0.8723 0.026 Uiso 1 1 calc R U .
C8 C 0.7571(2) 0.7307(2) 0.84209(7) 0.0199(5) Uani 1 1 d . . .
C9 C 0.7227(2) 0.6487(2) 0.81253(7) 0.0207(5) Uani 1 1 d . . .
C10 C 0.6247(3) 0.5420(3) 0.81579(8) 0.0277(6) Uani 1 1 d . . .
H10A H 0.5806 0.5229 0.8371 0.033 Uiso 1 1 calc R U .
C11 C 0.5918(3) 0.4641(3) 0.78809(9) 0.0327(7) Uani 1 1 d . . .
H11A H 0.5249 0.3918 0.7904 0.039 Uiso 1 1 calc R U .
C12 C 0.6559(3) 0.4909(3) 0.75686(8) 0.0287(6) Uani 1 1 d . . .
H12A H 0.6326 0.4371 0.7379 0.034 Uiso 1 1 calc R U .
C13 C 0.7545(2) 0.5968(2) 0.75330(7) 0.0208(5) Uani 1 1 d . . .
C14 C 0.7863(2) 0.6749(2) 0.78132(7) 0.0202(5) Uani 1 1 d . . .
H14A H 0.8529 0.7474 0.7790 0.024 Uiso 1 1 calc R U .
C15 C 0.8255(2) 0.6255(2) 0.72068(7) 0.0203(5) Uani 1 1 d . . .
C16 C 0.8317(3) 0.5580(2) 0.69415(7) 0.0224(6) Uani 1 1 d . . .
H16A H 0.7861 0.4778 0.6917 0.027 Uiso 1 1 calc R U .
C17 C 0.9200(2) 0.6335(2) 0.67152(7) 0.0222(6) Uani 1 1 d . . .
C18 C 0.9683(3) 0.6088(3) 0.63965(8) 0.0262(6) Uani 1 1 d . . .
C19 C 1.0790(3) 0.6843(3) 0.62955(9) 0.0360(8) Uani 1 1 d . . .
H19A H 1.1241 0.7537 0.6421 0.043 Uiso 1 1 calc R U .
C20 C 1.1214(4) 0.6543(5) 0.60018(12) 0.0560(13) Uani 1 1 d . . .
H20A H 1.1978 0.7032 0.5928 0.067 Uiso 1 1 calc R U .
C21 C 1.0550(5) 0.5554(5) 0.58178(11) 0.0632(15) Uani 1 1 d . . .
H21A H 1.0843 0.5352 0.5617 0.076 Uiso 1 1 calc R U .
C22 C 0.9463(5) 0.4870(4) 0.59298(9) 0.0501(12) Uani 1 1 d . . .
H22A H 0.8997 0.4194 0.5798 0.060 Uiso 1 1 calc R U .
P1 P 0.6667 0.3333 0.50073(5) 0.0501(5) Uani 1 3 d S T P
F1 F 0.7724(5) 0.3576(6) 0.52283(16) 0.189(3) Uani 1 1 d . . .
F2 F 0.7478(4) 0.4406(4) 0.47731(12) 0.1155(15) Uani 1 1 d . . .
O1 O 0.6667 0.3333 0.64352(12) 0.0378(9) Uani 1 3 d DS T P
H1 H 0.731(5) 0.389(6) 0.633(2) 0.057 Uiso 0.5 1 d D U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0211 0.0125
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
P P 0.1183 0.1134
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Br Br -0.7406 2.7887
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
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
N2 Fe1 N2 96.20(9) 3_675 .
N2 Fe1 N2 96.20(9) 3_675 2_765
N2 Fe1 N2 96.20(9) . 2_765
N2 Fe1 N1 89.16(9) 3_675 .
N2 Fe1 N1 80.33(10) . .
N2 Fe1 N1 173.92(10) 2_765 .
N2 Fe1 N1 80.33(10) 3_675 3_675
N2 Fe1 N1 173.92(10) . 3_675
N2 Fe1 N1 89.16(10) 2_765 3_675
N1 Fe1 N1 94.57(9) . 3_675
N2 Fe1 N1 173.92(10) 3_675 2_765
N2 Fe1 N1 89.16(10) . 2_765
N2 Fe1 N1 80.33(9) 2_765 2_765
N1 Fe1 N1 94.57(9) . 2_765
N1 Fe1 N1 94.57(9) 3_675 2_765
C1 N1 C5 117.3(2) . .
C1 N1 Fe1 127.4(2) . .
C5 N1 Fe1 115.33(18) . .
C6 N2 N3 106.5(2) . .
C6 N2 Fe1 116.45(18) . .
N3 N2 Fe1 136.88(19) . .
N2 N3 C8 110.7(2) . .
N2 N3 H3 124.6 . .
C8 N3 H3 124.6 . .
N5 N4 C15 111.7(2) . .
N5 N4 H4 124.2 . .
C15 N4 H4 124.2 . .
C17 N5 N4 105.7(2) . .
C18 N6 C22 116.5(4) . .
N1 C1 C2 122.7(3) . .
N1 C1 H1A 118.6 . .
C2 C1 H1A 118.6 . .
C3 C2 C1 119.7(3) . .
C3 C2 H2A 120.1 . .
C1 C2 H2A 120.1 . .
C2 C3 C4 118.4(3) . .
C2 C3 H3A 120.8 . .
C4 C3 H3A 120.8 . .
C5 C4 C3 118.9(3) . .
C5 C4 H4A 120.5 . .
C3 C4 H4A 120.5 . .
N1 C5 C4 122.8(3) . .
N1 C5 C6 112.7(2) . .
C4 C5 C6 124.5(3) . .
N2 C6 C7 110.3(2) . .
N2 C6 C5 114.9(2) . .
C7 C6 C5 134.8(3) . .
C8 C7 C6 104.8(2) . .
C8 C7 H7A 127.6 . .
C6 C7 H7A 127.6 . .
N3 C8 C7 107.6(2) . .
N3 C8 C9 121.9(2) . .
C7 C8 C9 130.5(3) . .
C14 C9 C10 119.1(3) . .
C14 C9 C8 121.1(3) . .
C10 C9 C8 119.8(3) . .
C11 C10 C9 120.2(3) . .
C11 C10 H10A 119.9 . .
C9 C10 H10A 119.9 . .
C10 C11 C12 120.4(3) . .
C10 C11 H11A 119.8 . .
C12 C11 H11A 119.8 . .
C11 C12 C13 120.1(3) . .
C11 C12 H12A 120.0 . .
C13 C12 H12A 120.0 . .
C14 C13 C12 118.9(3) . .
C14 C13 C15 120.3(3) . .
C12 C13 C15 120.8(3) . .
C9 C14 C13 121.3(3) . .
C9 C14 H14A 119.4 . .
C13 C14 H14A 119.4 . .
N4 C15 C16 107.0(2) . .
N4 C15 C13 121.3(2) . .
C16 C15 C13 131.7(3) . .
C15 C16 C17 105.1(3) . .
C15 C16 H16A 127.4 . .
C17 C16 H16A 127.4 . .
N5 C17 C16 110.4(2) . .
N5 C17 C18 120.3(3) . .
C16 C17 C18 129.3(3) . .
N6 C18 C19 123.5(3) . .
N6 C18 C17 117.0(3) . .
C19 C18 C17 119.5(3) . .
C18 C19 C20 117.0(4) . .
C18 C19 H19A 121.5 . .
C20 C19 H19A 121.5 . .
C21 C20 C19 121.1(4) . .
C21 C20 H20A 119.5 . .
C19 C20 H20A 119.5 . .
C22 C21 C20 118.3(3) . .
C22 C21 H21A 120.9 . .
C20 C21 H21A 120.9 . .
C21 C22 N6 123.7(4) . .
C21 C22 H22A 118.1 . .
N6 C22 H22A 118.1 . .
F1 P1 F1 94.0(4) 3_665 .
F1 P1 F1 94.0(4) 3_665 2_655
F1 P1 F1 94.0(4) . 2_655
F1 P1 F2 87.4(3) 3_665 3_665
F1 P1 F2 86.3(3) . 3_665
F1 P1 F2 178.6(4) 2_655 3_665
F1 P1 F2 178.6(3) 3_665 .
F1 P1 F2 87.4(3) . .
F1 P1 F2 86.3(3) 2_655 .
F2 P1 F2 92.3(3) 3_665 .
F1 P1 F2 86.3(3) 3_665 2_655
F1 P1 F2 178.6(4) . 2_655
F1 P1 F2 87.4(3) 2_655 2_655
F2 P1 F2 92.3(3) 3_665 2_655
F2 P1 F2 92.3(3) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.946(2) 3_675
Fe1 N2 1.946(2) .
Fe1 N2 1.946(2) 2_765
Fe1 N1 1.992(2) .
Fe1 N1 1.992(2) 3_675
Fe1 N1 1.992(2) 2_765
N1 C1 1.344(4) .
N1 C5 1.360(4) .
N2 C6 1.341(3) .
N2 N3 1.343(3) .
N3 C8 1.356(4) .
N3 H3 0.8800 .
N4 N5 1.348(3) .
N4 C15 1.349(4) .
N4 H4 0.8800 .
N5 C17 1.338(4) .
N6 C18 1.359(4) .
N6 C22 1.363(5) .
C1 C2 1.383(4) .
C1 H1A 0.9500 .
C2 C3 1.382(5) .
C2 H2A 0.9500 .
C3 C4 1.388(4) .
C3 H3A 0.9500 .
C4 C5 1.385(4) .
C4 H4A 0.9500 .
C5 C6 1.451(4) .
C6 C7 1.400(4) .
C7 C8 1.383(4) .
C7 H7A 0.9500 .
C8 C9 1.467(4) .
C9 C14 1.385(4) .
C9 C10 1.397(4) .
C10 C11 1.383(4) .
C10 H10A 0.9500 .
C11 C12 1.389(4) .
C11 H11A 0.9500 .
C12 C13 1.396(4) .
C12 H12A 0.9500 .
C13 C14 1.394(4) .
C13 C15 1.478(4) .
C14 H14A 0.9500 .
C15 C16 1.379(4) .
C16 C17 1.403(4) .
C16 H16A 0.9500 .
C17 C18 1.475(4) .
C18 C19 1.381(5) .
C19 C20 1.390(6) .
C19 H19A 0.9500 .
C20 C21 1.369(8) .
C20 H20A 0.9500 .
C21 C22 1.357(8) .
C21 H21A 0.9500 .
C22 H22A 0.9500 .
P1 F1 1.540(5) 3_665
P1 F1 1.540(5) .
P1 F1 1.540(5) 2_655
P1 F2 1.578(4) 3_665
P1 F2 1.578(4) .
P1 F2 1.578(4) 2_655
O1 H1 0.91(2) .
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
O1 H1 N6 0.91(2) 2.09(3) 2.969(4) 163(8)
N4 H4 Br1 0.88 2.60 3.453(2) 162.6
