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_4343548
_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                 100.627(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   44.373(3)
_cell_length_b                   7.9331(5)
_cell_length_c                   13.9724(9)
_cell_measurement_reflns_used    4983
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.80
_cell_volume                     4834.1(6)
_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      225(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1654
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -53
_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            34811
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.87
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.4708
_exptl_absorpt_correction_T_min  0.2101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0600P)^2^+12.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                2720
_reflns_number_total             4731
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic5b00546_si_002.cif
_cod_data_source_block           al17b_225
_cod_original_cell_volume        4834.1(5)
_cod_database_code               4343548
_olex2_refinement_description
;
1. Others
 Fixed U12: Co1(0)
 Fixed U23: Co1(0)
 Fixed Uiso: H4A(0.052) H4B(0.052) H5A(0.055) H5B(0.055) H6A(0.053) H6B(0.053)
 H7A(0.061) H7B(0.061) H8A(0.061) H8B(0.061) H9A(0.068) H9B(0.068) H10A(0.061)
 H10B(0.061) H11A(0.073) H11B(0.073) H12A(0.064) H12B(0.064) H13A(0.074)
 H13B(0.074) H14A(0.068) H14B(0.068) H15A(0.075) H15B(0.075) H16A(0.068)
 H16B(0.068) H17A(0.075) H17B(0.075) H18A(0.08) H18B(0.08) H19A(0.108)
 H19B(0.108) H19C(0.108)
 Fixed X: Co1(0) H4A(0.1169) H4B(0.1143) H5A(0.1141) H5B(0.1036) H6A(0.164)
 H6B(0.154) H7A(0.1573) H7B(0.144) H8A(0.2061) H8B(0.193) H9A(0.198)
 H9B(0.1839) H10A(0.2462) H10B(0.2321) H11A(0.2375) H11B(0.2236) H12A(0.2859)
 H12B(0.272) H13A(0.2772) H13B(0.2638) H14A(0.3258) H14B(0.3124) H15A(0.3172)
 H15B(0.3039) H16A(0.3659) H16B(0.353) H17A(0.356) H17B(0.3427) H18A(0.4049)
 H18B(0.3923) H19A(0.4153) H19B(0.3919) H19C(0.3801)
 Fixed Y: H4A(0.5565) H4B(0.3736) H5A(0.6801) H5B(0.5103) H6A(0.5765)
 H6B(0.3984) H7A(0.6974) H7B(0.5271) H8A(0.5735) H8B(0.4014) H9A(0.6995)
 H9B(0.5302) H10A(0.5686) H10B(0.3991) H11A(0.6974) H11B(0.5273) H12A(0.5669)
 H12B(0.398) H13A(0.698) H13B(0.5276) H14A(0.5714) H14B(0.402) H15A(0.7041)
 H15B(0.5341) H16A(0.5847) H16B(0.4108) H17A(0.7066) H17B(0.5339) H18A(0.5952)
 H18B(0.4155) H19A(0.5455) H19B(0.6975) H19C(0.5157)
 Fixed Z: Co1(0.25) H4A(0.3252) H4B(0.2795) H5A(0.1771) H5B(0.1217)
 H6A(0.2247) H6B(0.1787) H7A(0.0731) H7B(0.0238) H8A(0.1156) H8B(0.0684) H9A(-
 0.0369) H9B(-0.085) H10A(0.0042) H10B(-0.0439) H11A(-0.1484) H11B(-0.1962)
 H12A(-0.1064) H12B(-0.1556) H13A(-0.2585) H13B(-0.3071) H14A(-0.2162) H14B(-
 0.2661) H15A(-0.3676) H15B(-0.4172) H16A(-0.3286) H16B(-0.3737) H17A(-0.4822)
 H17B(-0.5276) H18A(-0.4483) H18B(-0.4849) H19A(-0.601) H19B(-0.6072) H19C(-
 0.6432)
;