β-Fluorinated porpholactones and metal complexes: synthesis, characterization and some spectroscopic studies
Hu, Ji-Yun; Wu, Zhuo-Yan; Chai, Ke; Yang, Zi-Shu; Meng, Yin-Shan; Ning, Yingying; Zhang, Jing; Zhang, Jun-Long; Inorganic Chemistry Frontiers 4 (2017) 1539–; doi:10.1039/C7QI00375G

data_4349760
_publ_section_title
;
 \b-Fluorinated porpholactones and metal complexes: synthesis,
 characterization and some spectroscopic studies
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1539
_journal_paper_doi               10.1039/C7QI00375G
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C29.5 H9 Cl3 F13 N4 O Zn0.5'
_chemical_formula_weight         821.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-03-25 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                92.344(3)
_cell_angle_beta                 100.789(4)
_cell_angle_gamma                103.221(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5290(5)
_cell_length_b                   11.8506(4)
_cell_length_c                   12.6670(5)
_cell_measurement_reflns_used    5092
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.6910
_cell_measurement_theta_min      3.1300
_cell_volume                     1505.63(11)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20287
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.855
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       plate
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.3045
_exptl_crystal_size_mid          0.2750
_exptl_crystal_size_min          0.0534
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0875
_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^)+(0.1206P)^2^+4.4914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2409
_refine_ls_wR_factor_ref         0.2603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4093
_reflns_number_total             5312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00375g2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C29.50 H9 Cl3 F13 N4 O Zn0.50'
_cod_database_code               4349760
_shelxl_version_number           2014-3
_shelx_res_checksum              74864
_shelx_hkl_checksum              55985