Synthesis and Temperature-Induced Structural Phase and Spin Transitions in Hexadecylboron-Capped Cobalt(II) Hexachloroclathrochelate and Its Diamagnetic Iron(II)-Encapsulating Analogue.
Vologzhanina, Anna V.; Belov, Alexander S.; Novikov, Valentin V.; Dolganov, Alexander V.; Romanenko, Galina V.; Ovcharenko, Victor I.; Korlyukov, Alexander A.; Buzin, Mikhail I.; Voloshin, Yan Z.; Inorganic chemistry 54 (2015) 5827–5838; doi:10.1021/acs.inorgchem.5b00546

data_4343538
_publ_section_title
;
 Synthesis and Temperature-Induced Structural Phase and Spin Transitions
 in Hexadecylboron-Capped Cobalt(II) Hexachloroclathrochelate and Its
 Diamagnetic Iron(II)-Encapsulating Analogue.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5827
_journal_page_last               5838
_journal_paper_doi               10.1021/acs.inorgchem.5b00546
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C38 H66 B2 Cl6 Fe N6 O6'
_chemical_formula_sum            'C38 H66 B2 Cl6 Fe N6 O6'
_chemical_formula_weight         993.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 102.504(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   44.739(4)
_cell_length_b                   7.8988(8)
_cell_length_c                   13.8864(14)
_cell_measurement_reflns_used    2253
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.80
_cell_volume                     4790.8(8)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1101
_diffrn_reflns_av_unetI/netI     0.1108
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17047
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.3792
_exptl_absorpt_correction_T_min  0.2255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                2614
_reflns_number_total             4706
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic5b00546_si_002.cif
_cod_data_source_block           al14_168
_cod_original_cell_volume        4790.9(8)
_cod_database_code               4343538
_olex2_refinement_description
;
1. Others
 Fixed U12: Fe1(0)
 Fixed U23: Fe1(0)
 Fixed Uiso: H4A(0.038) H4B(0.038) H5A(0.041) H5B(0.041) H6A(0.042) H6B(0.042)
 H7A(0.046) H7B(0.046) H8A(0.044) H8B(0.044) H9A(0.048) H9B(0.048) H10A(0.046)
 H10B(0.046) H11A(0.049) H11B(0.049) H12A(0.045) H12B(0.045) H13A(0.05)
 H13B(0.05) H14A(0.05) H14B(0.05) H15A(0.05) H15B(0.05) H16A(0.053) H16B(0.053)
 H17A(0.053) H17B(0.053) H18A(0.056) H18B(0.056) H19A(0.082) H19B(0.082)
 H19C(0.082)
 Fixed X: Fe1(0) H4A(0.1156) H4B(0.1132) H5A(0.1018) H5B(0.1091) H6A(0.1538)
 H6B(0.1603) H7A(0.1416) H7B(0.1488) H8A(0.2007) H8B(0.1938) H9A(0.1875)
 H9B(0.1808) H10A(0.2333) H10B(0.2398) H11A(0.2205) H11B(0.2261) H12A(0.2786)
 H12B(0.2729) H13A(0.265) H13B(0.2601) H14A(0.3128) H14B(0.3177) H15A(0.3041)
 H15B(0.3001) H16A(0.3531) H16B(0.357) H17A(0.3391) H17B(0.3428) H18A(0.3924)
 H18B(0.3959) H19A(0.4101) H19B(0.3792) H19C(0.3781)
 Fixed Y: H4A(0.5642) H4B(0.3705) H5A(0.4701) H5B(0.6578) H6A(0.3947)
 H6B(0.5899) H7A(0.4681) H7B(0.662) H8A(0.5965) H8B(0.4005) H9A(0.6576)
 H9B(0.4614) H10A(0.4004) H10B(0.5972) H11A(0.4551) H11B(0.6528) H12A(0.5996)
 H12B(0.402) H13A(0.6529) H13B(0.4545) H14A(0.4079) H14B(0.6063) H15A(0.6556)
 H15B(0.4565) H16A(0.4182) H16B(0.6179) H17A(0.4607) H17B(0.6604) H18A(0.4263)
 H18B(0.6268) H19A(0.5536) H19B(0.6619) H19C(0.4604)
 Fixed Z: Fe1(0.25) H4A(0.3372) H4B(0.3026) H5A(0.133) H5B(0.1742) H6A(0.2066)
 H6B(0.2343) H7A(0.0361) H7B(0.0647) H8A(0.1248) H8B(0.1014) H9A(-0.0461) H9B(-
 0.0692) H10A(-0.0061) H10B(0.0154) H11A(-0.1776) H11B(-0.1571) H12A(-0.0934)
 H12B(-0.1142) H13A(-0.265) H13B(-0.2849) H14A(-0.2206) H14B(-0.2012) H15A(-
 0.3738) H15B(-0.3922) H16A(-0.3271) H16B(-0.3107) H17A(-0.4996) H17B(-0.4835)
 H18A(-0.4381) H18B(-0.4236) H19A(-0.5708) H19B(-0.5985) H19C(-0.6104)
;