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_7225924
_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 H41 Cd N3 O12, H2O'
_chemical_formula_sum            'C45 H43 Cd N3 O13'
_chemical_formula_weight         960.21
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-06 deposited with the CCDC.
2016-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                73.5850(10)
_cell_angle_beta                 87.9210(10)
_cell_angle_gamma                71.4450(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6126(2)
_cell_length_b                   13.5051(2)
_cell_length_c                   14.6564(3)
_cell_measurement_reflns_used    7175
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      58.52
_cell_measurement_theta_min      3.15
_cell_volume                     2266.30(7)
_computing_cell_refinement
;       
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.903
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9224
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        58.741
_diffrn_reflns_theta_max         58.741
_diffrn_reflns_theta_min         3.149
_exptl_absorpt_coefficient_mu    4.443
_exptl_absorpt_correction_T_max  1.00000
_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            yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         5819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0729P)^2^+0.6065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5567
_reflns_number_total             5819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01231k2.cif
_cod_data_source_block           jd091_0m
_cod_depositor_comments
'Adding full bibliography for 7225922--7225924.cif.'
_cod_database_code               7225924
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.403
_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
2. Others
 Fixed Sof: O015(0.5) O01D(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00G(H00G), C00I(H00I), C00N(H00N), C00Q(H00Q), C00S(H00S),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C010(H010), C016(H016), C018(H018),
 C019(H019), C01B(H01D), C01G(H01K), C01H(H01L), C01I(H01M), C01J(H01N),
 C01K(H01O), C01M(H01S), C01N(H01T), C01O(H01U), C01P(H01V), C01Q(H01W),
 C01R(H01X)
3.b Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C01E(H01E,H01F,H01G), C01F(H01H,H01I,H01J), C01L(H01P,
 H01Q,H01R)
3.c Idealised tetrahedral OH refined as rotating group:
 O006(H006), O008(H008), O009(H009), O00F(H00F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'