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_4343543
_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 Co N6 O6'
_chemical_formula_sum            'C38 H66 B2 Cl6 Co N6 O6'
_chemical_formula_weight         996.22
_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                 101.225(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.99(2)
_cell_length_b                   7.938(4)
_cell_length_c                   13.853(8)
_cell_measurement_reflns_used    1716
_cell_measurement_temperature    40(2)
_cell_measurement_theta_max      19.58
_cell_measurement_theta_min      2.93
_cell_volume                     4745(4)
_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      40(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1611
_diffrn_reflns_av_unetI/netI     0.1800
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13674
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.3679
_exptl_absorpt_correction_T_min  0.2770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4596
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1759
_reflns_number_gt                2329
_reflns_number_total             4596
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic5b00546_si_002.cif
_cod_data_source_block           al17a_40
_cod_database_code               4343543
_olex2_refinement_description
;
1. Others
 Fixed U12: Co1(0)
 Fixed U23: Co1(0)
 Fixed Uiso: H4A(0.027) H4B(0.027) H5A(0.03) H5B(0.03) H6A(0.031) H6B(0.031)
 H7A(0.033) H7B(0.033) H8A(0.034) H8B(0.034) H9A(0.034) H9B(0.034) H10A(0.035)
 H10B(0.035) H11A(0.037) H11B(0.037) H12A(0.035) H12B(0.035) H13A(0.034)
 H13B(0.034) H14A(0.036) H14B(0.036) H15A(0.034) H15B(0.034) H16A(0.034)
 H16B(0.034) H17A(0.033) H17B(0.033) H18A(0.032) H18B(0.032) H19A(0.046)
 H19B(0.046) H19C(0.046)
 Fixed X: Co1(0) H4A(0.1177) H4B(0.1157) H5A(0.104) H5B(0.1156) H6A(0.1542)
 H6B(0.1655) H7A(0.1438) H7B(0.1583) H8A(0.2074) H8B(0.1929) H9A(0.1989)
 H9B(0.1836) H10A(0.2321) H10B(0.2473) H11A(0.2235) H11B(0.2384) H12A(0.272)
 H12B(0.287) H13A(0.2637) H13B(0.2783) H14A(0.3122) H14B(0.3269) H15A(0.3036)
 H15B(0.3189) H16A(0.3674) H16B(0.3523) H17A(0.3592) H17B(0.3421) H18A(0.3902)
 H18B(0.4069) H19A(0.4148) H19B(0.3979) H19C(0.3782)
 Fixed Y: H4A(0.5771) H4B(0.3912) H5A(0.5291) H5B(0.6992) H6A(0.4108)
 H6B(0.5875) H7A(0.5504) H7B(0.7192) H8A(0.5849) H8B(0.4152) H9A(0.7228)
 H9B(0.5554) H10A(0.4163) H10B(0.5844) H11A(0.5538) H11B(0.7227) H12A(0.4166)
 H12B(0.5839) H13A(0.5572) H13B(0.7255) H14A(0.4212) H14B(0.5895) H15A(0.5634)
 H15B(0.7298) H16A(0.5919) H16B(0.4229) H17A(0.7283) H17B(0.5649) H18A(0.4134)
 H18B(0.5822) H19A(0.5351) H19B(0.7117) H19C(0.5529)
 Fixed Z: Co1(0.25) H4A(0.3271) H4B(0.2821) H5A(0.1192) H5B(0.1761)
 H6A(0.1748) H6B(0.2248) H7A(0.0161) H7B(0.0689) H8A(0.1128) H8B(0.0608) H9A(-
 0.0413) H9B(-0.0939) H10A(-0.052) H10B(-0.0003) H11A(-0.2073) H11B(-0.1557)
 H12A(-0.1652) H12B(-0.1119) H13A(-0.3194) H13B(-0.2665) H14A(-0.2756) H14B(-
 0.2227) H15A(-0.4302) H15B(-0.3767) H16A(-0.3367) H16B(-0.3874) H17A(-0.4902)
 H17B(-0.5423) H18A(-0.5022) H18B(-0.456) H19A(-0.6206) H19B(-0.6119) H19C(-
 0.66)
;