Temperature-Dependent in Situ Ligand Cyclization via C=C Coupling and Formation of a Spin-Crossover Iron(II) Coordination Polymer
Feng-Lei Yang; Jun Tao; Rong-Bin Huang; Lan-Sun Zheng; Inorganic Chemistry 50 (2011) 911–917; doi:10.1021/ic101490a

data_4324306
_publ_contact_author_address
;
Department of Chemistry
Xiamen University
Xiamen 361005
P. R. China
;
_publ_contact_author_email       taojun@xmu.edu.cn
_publ_contact_author_name        'Prof. Jun Tao'
_publ_contact_author_phone       86-592-2188138
_publ_section_title
;
 Temperature-Dependent in Situ Ligand Cyclization via C=C Coupling and
 Formation of a Spin-Crossover Iron(II) Coordination Polymer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              911
_journal_page_last               917
_journal_paper_doi               10.1021/ic101490a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H28 Fe N10 O S2'
_chemical_formula_weight         664.59
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.549(2)
_cell_length_b                   12.5168(8)
_cell_length_c                   18.6829(11)
_cell_measurement_reflns_used    2951
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.8717
_cell_measurement_theta_min      2.7608
_cell_volume                     6910.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w 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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.1412
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11669
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.81
_diffrn_standards_number         12719
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.8902
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6601
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                3853
_reflns_number_total             6601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101490a_si_001_6.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        6909.9(8)
_cod_database_code               4324306