Synthesis, structure, and spin crossover above room temperature of a mononuclear and related dinuclear double helicate iron(ii) complexes.
Hagiwara, Hiroaki; Tanaka, Tomoko; Hora, Shiori; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17132–17140; doi:10.1039/c6dt02766k

data_7040296
_publ_section_title
;
 Synthesis, structure, and spin crossover above room temperature of a
 mononuclear and related dinuclear double helicate iron(ii) complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17132
_journal_page_last               17140
_journal_paper_doi               10.1039/c6dt02766k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C46 H51 F18 Fe2 N21 P3'
_chemical_formula_weight         1444.68
_chemical_properties_physical    ', Efflorescent'
_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_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-08-09 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.907(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.932(8)
_cell_length_b                   20.020(5)
_cell_length_c                   11.614(3)
_cell_measurement_reflns_used    6709
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4775
_cell_measurement_theta_min      3.1299
_cell_volume                     6844(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare, et al., 1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26200
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.130
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.8419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             2932
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/acetonitrile'
_exptl_crystal_size_max          0.4000
_exptl_crystal_size_mid          0.3800
_exptl_crystal_size_min          0.0700
_platon_squeeze_details
; 
The PLATON SQUEEZE program was used to treat regions having highly disordered solvent molecules and counter anions which could not be sensibly modelled in terms of atomic sites. Available void volume is 1386.1 \%A^3^. 473 electrons per unit cell were located and these were assigned to 1 PF6 and 5 H2O molecules per complex [473/4 = 119 e per complex; PF6 (69) + 5 H2O (10) = 119 electrons].
;
_refine_diff_density_max         0.647
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+64.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4176
_reflns_number_total             7826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02766k2.cif
_cod_data_source_block           Dinuclear_2_120K_SQUEEZE
_cod_depositor_comments
'Adding full bibliography for 7040294--7040296.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7040296
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.960
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              69232