Fluorescence of a triple-stranded helicate iron(iii) complex from a novel bis-β-diketone ligand: synthesis, structure and spectroscopic studies
Zou, Fang; Tang, Xiao; Huang, Yuhong; Wan, Shigang; Lu, Fa; Chen, Zhe-Ning; Wu, Anan; Zhang, Hui; CrystEngComm 18 (2016) 6624–; doi:10.1039/C6CE01231K

data_7225923
_publ_section_title
;
 Fluorescence of a triple-stranded helicate iron(iii) complex from a novel
 bis-\b-diketone ligand: synthesis, structure and spectroscopic studies
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6624
_journal_paper_doi               10.1039/C6CE01231K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety
'C45 H36 Fe2 O18, 4(H2 O), 4(C4 H8 O), C5 H5 N'
_chemical_formula_sum            'C65 H81 Fe2 N O26'
_chemical_formula_weight         1416.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-07-09
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.05.11 svn.r3296 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2016-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                111.6570(10)
_cell_angle_beta                 101.8720(10)
_cell_angle_gamma                108.4520(10)
_cell_formula_units_Z            2
_cell_length_a                   14.2812(2)
_cell_length_b                   16.2445(2)
_cell_length_c                   18.4229(3)
_cell_measurement_reflns_used    4955
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      58.547
_cell_measurement_theta_min      3.587
_cell_volume                     3506.82(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.808
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.808
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12783
_diffrn_reflns_point_group_measured_fraction_full 0.808
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        58.783
_diffrn_reflns_theta_max         58.783
_diffrn_reflns_theta_min         3.587
_exptl_absorpt_coefficient_mu    3.979
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.33698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             1442
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
SQUEEZE removed 4 disordered tetrahyfrofuran, 
2 disordered water molecules and 0ne pyridine molecule per formula unit.
;
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8084
_refine_ls_number_restraints     615
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+2.4208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6851
_reflns_number_total             8084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01231k2.cif
_cod_data_source_block           p1_sq
_cod_depositor_comments
'Adding full bibliography for 7225922--7225924.cif.'
_cod_original_cell_volume        3506.82(9)
_cod_original_formula_sum        'C65 H81 Fe2 N O26 '
_cod_database_code               7225923
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Rigid bond restraints
 O008, C00Z
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 O00D, C01D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C00M, C013
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Free rotating group:
 O00H(H00A,H00B), O018(H01Z,H)
4.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00R(H00R), C00T(H00T), C00V(H00V), C00W(H00W), C013(H013),
 C019(H019), C01A(H01A), C01C(H01C), C01F(H01F), C01G(H01G), C01I(H01I),
 C01J(H01J), C01K(H01K), C01N(H01N)
4.c Idealised Me refined as rotating group:
 C01L(H01B,H01D,H01E), C01R(H01H,H01L,H01M), C01S(H01O,H01P,H01Q), C01T(H01R,
 H01S,H01T), C01U(H01U,H01V,H01W), C01V(H01X,H01Y,HA)
4.d Idealised tetrahedral OH refined as rotating group:
 O00F(H00F), O00L(H00L), O00N(H00N)
;
_shelx_res_checksum              82879
_shelx_fab_checksum              38900
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20