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
Daniel L. Reger; Christine A. Little; Mark D. Smith; Gary J. Long; Inorganic Chemistry 41 (2002) 4453–4460; doi:10.1021/ic0112645

data_4318355
_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 F8 N12 Ni'
_chemical_formula_weight         829.12
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.130(9)
_cell_angle_beta                 104.627(5)
_cell_angle_gamma                116.302(11)
_cell_formula_units_Z            2
_cell_length_a                   10.261(4)
_cell_length_b                   11.327(4)
_cell_length_c                   18.952(7)
_cell_measurement_reflns_used    2312
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.246
_cell_measurement_theta_min      2.686
_cell_volume                     1888.6(12)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.624 (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      125(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1364
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7992
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.079
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.169
_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   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7992
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0897
_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/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                4618
_reflns_number_total             7992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112645_4.cif
_cod_data_source_block           ni125k
_cod_original_cell_volume        1888.4(11)
_cod_database_code               4318355