A temperature-dependent order-disorder and crystallographic phase transition in a 0D Fe(ii) spin crossover compound and its non-spin crossover Co(ii) isomorph.
Ross, Tamsyn M.; Moubaraki, Boujemaa; Wallwork, Kia S.; Batten, Stuart R.; Murray, Keith S.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 10147–10155; doi:10.1039/c1dt10961h

data_7016900
_publ_section_title
;
 A temperature-dependent order-disorder and crystallographic phase
 transition in a 0D Fe(ii) spin crossover compound and its non-spin
 crossover Co(ii) isomorph.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10147
_journal_page_last               10155
_journal_paper_doi               10.1039/c1dt10961h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C44 H62 B2 Fe N18'
_chemical_formula_sum            'C44 H62 B2 Fe N18'
_chemical_formula_weight         920.59
_chemical_name_common            '[Fe(II)(NCBH3)2(DDE)2]'
_chemical_name_systematic
;
[Fe(II)(NCBH3)2(DDE)2]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 92.445(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5660(10)
_cell_length_b                   13.756(2)
_cell_length_c                   17.1800(10)
_cell_measurement_reflns_used    52078
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      1.61
_cell_volume                     4855.9(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.77502
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52078
_diffrn_reflns_theta_full        26.21
_diffrn_reflns_theta_max         26.21
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9964
_exptl_absorpt_correction_T_min  0.9821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0137(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         7369
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0764P)^2^+12.1614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                6462
_reflns_number_total             7369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10961h.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7016900