#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:47:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179263 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/83/4318352.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_4318352
loop_
_publ_author_name
'Daniel L. Reger'
'Christine A. Little'
'Mark D. Smith'
'Gary J. Long'
_publ_section_title
;
 Solid-State Structural and Magnetic Investigations of
 {M[HC(3,5-Me2pz)3]2}(BF4)2 (M = Fe, Co, Ni, Cu): Observation of a
 Thermally Induced Solid-State Phase Change Controlling an Iron(II)
 Spin-State Crossover
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4453
_journal_page_last               4460
_journal_paper_doi               10.1021/ic0112645
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H44 B2 Co F8 N12'
_chemical_formula_weight         829.34
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 111.4640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3012(12)
_cell_length_b                   10.3039(6)
_cell_length_c                   19.6375(12)
_cell_measurement_reflns_used    6065
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      26.371
_cell_measurement_theta_min      2.229
_cell_volume                     3822.9(4)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16977
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0437
_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)+(0.0575P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                2874
_reflns_number_total             3918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112645_1.cif
_cod_data_source_block           co220k
_cod_database_code               4318352
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Co Co 0.5000 0.0000 1.0000 0.02527(14) Uani 1 2 d S . .
C1 C 0.42092(12) 0.2205(2) 0.89265(12) 0.0257(5) Uani 1 1 d . . .
H1 H 0.3959(10) 0.2869(18) 0.8590(11) 0.009(5) Uiso 1 1 d . . .
C11 C 0.35813(13) 0.3166(2) 0.97065(13) 0.0321(6) Uani 1 1 d . . .
C12 C 0.36222(15) 0.2907(3) 1.04016(14) 0.0438(7) Uani 1 1 d . . .
H12 H 0.3369 0.3325 1.0654 0.053 Uiso 1 1 calc R . .
C13 C 0.41109(15) 0.1905(3) 1.06677(14) 0.0417(7) Uani 1 1 d . . .
C14 C 0.31484(14) 0.4128(3) 0.91678(15) 0.0442(7) Uani 1 1 d . . .
H14A H 0.3452 0.4639 0.8988 0.066 Uiso 1 1 calc R . .
H14B H 0.2912 0.4696 0.9401 0.066 Uiso 1 1 calc R . .
H14C H 0.2797 0.3679 0.8762 0.066 Uiso 1 1 calc R . .
C15 C 0.4353(2) 0.1285(3) 1.14120(16) 0.0712(11) Uani 1 1 d . . .
H15A H 0.3974 0.0759 1.1455 0.107 Uiso 1 1 calc R . .
H15B H 0.4481 0.1955 1.1785 0.107 Uiso 1 1 calc R . .
H15C H 0.4762 0.0741 1.1477 0.107 Uiso 1 1 calc R . .
C21 C 0.35655(12) 0.0746(2) 0.78562(12) 0.0299(5) Uani 1 1 d . . .
C22 C 0.35033(13) -0.0575(3) 0.77946(13) 0.0371(6) Uani 1 1 d . . .
H22 H 0.3250 -0.1045 0.7369 0.045 Uiso 1 1 calc R . .
C23 C 0.38854(13) -0.1089(2) 0.84812(14) 0.0381(6) Uani 1 1 d . . .
C24 C 0.32723(15) 0.1789(3) 0.73047(13) 0.0434(7) Uani 1 1 d . . .
H24A H 0.3019 0.2412 0.7488 0.065 Uiso 1 1 calc R . .
H24B H 0.2951 0.1413 0.6853 0.065 Uiso 1 1 calc R . .
H24C H 0.3656 0.2224 0.7214 0.065 Uiso 1 1 calc R . .
C25 C 0.39701(18) -0.2485(2) 0.87001(17) 0.0634(10) Uani 1 1 d . . .
H25A H 0.4328 -0.2567 0.9187 0.095 Uiso 1 1 calc R . .
H25B H 0.4114 -0.2975 0.8356 0.095 Uiso 1 1 calc R . .
H25C H 0.3523 -0.2820 0.8700 0.095 Uiso 1 1 calc R . .
C31 C 0.52975(13) 0.3370(2) 0.89048(14) 0.0344(6) Uani 1 1 d . . .
C32 C 0.59986(14) 0.3065(3) 0.91823(15) 0.0413(7) Uani 1 1 d . . .
H32 H 0.6370 0.3556 0.9136 0.050 Uiso 1 1 calc R . .
C33 C 0.60600(13) 0.1882(3) 0.95483(15) 0.0404(6) Uani 1 1 d . . .
C34 C 0.49177(16) 0.4512(3) 0.84755(19) 0.0599(9) Uani 1 1 d . . .
H34A H 0.4585 0.4224 0.8005 0.090 Uiso 1 1 calc R . .
H34B H 0.5257 0.5103 0.8401 0.090 Uiso 1 1 calc R . .
H34C H 0.4664 0.4953 0.8741 0.090 Uiso 1 1 calc R . .
C35 C 0.67207(15) 0.1142(3) 0.9949(2) 0.0668(10) Uani 1 1 d . . .
H35A H 0.7005 0.1621 1.0382 0.100 Uiso 1 1 calc R . .
H35B H 0.6988 0.1022 0.9633 0.100 Uiso 1 1 calc R . .
H35C H 0.6599 0.0301 1.0092 0.100 Uiso 1 1 calc R . .
N11 N 0.43687(11) 0.15359(19) 1.01623(10) 0.0329(5) Uani 1 1 d . . .
N12 N 0.40364(10) 0.23255(17) 0.95739(10) 0.0267(4) Uani 1 1 d . . .
N21 N 0.41848(11) -0.01449(18) 0.89579(11) 0.0331(5) Uani 1 1 d . . .
N22 N 0.39798(10) 0.09809(17) 0.85660(10) 0.0271(4) Uani 1 1 d . . .
N31 N 0.54260(10) 0.14624(19) 0.95056(11) 0.0332(5) Uani 1 1 d . . .
N32 N 0.49612(10) 0.23887(18) 0.91023(10) 0.0282(4) Uani 1 1 d . . .
B B 0.31691(16) 0.5604(3) 0.69537(16) 0.0380(7) Uani 1 1 d . . .
F1 F 0.31730(9) 0.50442(15) 0.75949(8) 0.0510(4) Uani 1 1 d . . .
F2 F 0.29323(12) 0.47368(19) 0.63932(10) 0.0797(6) Uani 1 1 d . . .
F3 F 0.38517(9) 0.5974(2) 0.70479(9) 0.0735(6) Uani 1 1 d . . .
F4 F 0.27479(10) 0.66772(17) 0.67885(10) 0.0703(5) Uani 1 1 d . . .
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
N21 Co N21 180.000(1) 5_657 . ?
N21 Co N11 84.07(8) 5_657 5_657 ?
N21 Co N11 95.93(8) . 5_657 ?
N21 Co N11 95.93(8) 5_657 . ?
N21 Co N11 84.07(8) . . ?
N11 Co N11 180.00(10) 5_657 . ?
N21 Co N31 85.05(8) 5_657 5_657 ?
N21 Co N31 94.95(8) . 5_657 ?
N11 Co N31 84.84(8) 5_657 5_657 ?
N11 Co N31 95.16(8) . 5_657 ?
N21 Co N31 94.95(8) 5_657 . ?
N21 Co N31 85.05(8) . . ?
N11 Co N31 95.16(8) 5_657 . ?
N11 Co N31 84.84(8) . . ?
N31 Co N31 180.0 5_657 . ?
N22 C1 N12 111.73(18) . . ?
N22 C1 N32 110.83(18) . . ?
N12 C1 N32 110.69(18) . . ?
N12 C11 C12 105.7(2) . . ?
N12 C11 C14 123.8(2) . . ?
C12 C11 C14 130.5(2) . . ?
C11 C12 C13 107.1(2) . . ?
N11 C13 C12 110.5(2) . . ?
N11 C13 C15 121.6(2) . . ?
C12 C13 C15 127.9(2) . . ?
N22 C21 C22 105.7(2) . . ?
N22 C21 C24 123.4(2) . . ?
C22 C21 C24 131.0(2) . . ?
C21 C22 C23 107.0(2) . . ?
N21 C23 C22 110.6(2) . . ?
N21 C23 C25 121.7(2) . . ?
C22 C23 C25 127.7(2) . . ?
N32 C31 C32 106.0(2) . . ?
N32 C31 C34 122.8(2) . . ?
C32 C31 C34 131.2(2) . . ?
C31 C32 C33 106.9(2) . . ?
N31 C33 C32 110.4(2) . . ?
N31 C33 C35 121.9(2) . . ?
C32 C33 C35 127.6(2) . . ?
C13 N11 N12 104.57(19) . . ?
C13 N11 Co 137.96(17) . . ?
N12 N11 Co 116.83(14) . . ?
C11 N12 N11 112.06(18) . . ?
C11 N12 C1 128.72(19) . . ?
N11 N12 C1 119.20(18) . . ?
C23 N21 N22 104.89(19) . . ?
C23 N21 Co 136.52(16) . . ?
N22 N21 Co 116.95(14) . . ?
C21 N22 N21 111.80(18) . . ?
C21 N22 C1 128.92(19) . . ?
N21 N22 C1 119.27(18) . . ?
C33 N31 N32 104.80(19) . . ?
C33 N31 Co 137.94(17) . . ?
N32 N31 Co 116.44(14) . . ?
C31 N32 N31 111.87(19) . . ?
C31 N32 C1 128.86(19) . . ?
N31 N32 C1 119.25(18) . . ?
F2 B F4 109.6(2) . . ?
F2 B F1 110.2(2) . . ?
F4 B F1 110.5(2) . . ?
F2 B F3 109.2(2) . . ?
F4 B F3 108.6(3) . . ?
F1 B F3 108.8(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co N21 2.1143(19) 5_657 ?
Co N21 2.1143(19) . ?
Co N11 2.1326(19) 5_657 ?
Co N11 2.1326(19) . ?
Co N31 2.1390(19) 5_657 ?
Co N31 2.1390(19) . ?
C1 N22 1.437(3) . ?
C1 N12 1.443(3) . ?
C1 N32 1.449(3) . ?
C11 N12 1.359(3) . ?
C11 C12 1.363(3) . ?
C11 C14 1.481(3) . ?
C12 C13 1.394(4) . ?
C13 N11 1.335(3) . ?
C13 C15 1.503(4) . ?
C21 N22 1.361(3) . ?
C21 C22 1.367(3) . ?
C21 C24 1.487(3) . ?
C22 C23 1.391(3) . ?
C23 N21 1.333(3) . ?
C23 C25 1.493(3) . ?
C31 N32 1.354(3) . ?
C31 C32 1.362(4) . ?
C31 C34 1.488(3) . ?
C32 C33 1.397(4) . ?
C33 N31 1.331(3) . ?
C33 C35 1.493(4) . ?
N11 N12 1.372(2) . ?
N21 N22 1.370(2) . ?
N31 N32 1.372(2) . ?
B F2 1.361(3) . ?
B F4 1.363(3) . ?
B F1 1.382(3) . ?
B F3 1.383(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co N31 N32 C31 170.84(16) . . . . ?
Co N21 N22 C21 167.28(15) . . . . ?
Co N11 N12 C11 172.41(15) . . . . ?
