Functionalized pyridine in pyclen-based iron(iii) complexes: evaluation of fundamental properties
Mekhail, Magy A.; Pota, Kristof; Schwartz, Timothy M.; Green, Kayla N.; RSC Advances 10 (2020) 31165–31170; doi:10.1039/D0RA05756H

data_7241137
_publ_section_title
;
 Functionalized pyridine in pyclen-based iron(iii) complexes: evaluation
 of fundamental properties
;
_journal_issue                   52
_journal_name_full               'RSC Advances'
_journal_page_first              31165
_journal_page_last               31170
_journal_paper_doi               10.1039/D0RA05756H
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C12 H17 Cl2 F3 Fe N4, C F3 O3 S'
_chemical_formula_sum            'C13 H17 Cl2 F6 Fe N4 O3 S'
_chemical_formula_weight         550.112
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_Int_Tables_number      11
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-13
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.751(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9632(3)
_cell_length_b                   10.2625(5)
_cell_length_c                   14.6539(7)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      29.616
_cell_measurement_theta_min      2.806
_cell_volume                     1037.60(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            84300
_diffrn_reflns_point_group_measured_fraction_full 0.9985
_diffrn_reflns_point_group_measured_fraction_max 0.9955
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       prism
_exptl_crystal_F_000             555.922
_exptl_crystal_size_max          0.852
_exptl_crystal_size_mid          0.542
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.7224
_refine_diff_density_min         -0.4106
_refine_diff_density_rms         0.0970
_refine_ls_d_res_high            0.7182
_refine_ls_d_res_low             7.2600
_refine_ls_goodness_of_fit_ref   1.0543
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0543
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+1.7621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2802
_reflns_number_total             3075
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ra05756h2.cif
_cod_data_source_block           MM_II_011120_FeL10_0m
_cod_depositor_comments
'Adding full bibliography for 7241133--7241138.cif.'
_cod_database_code               7241137
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C3(H3a,H3b), C2(H2a,H2b)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'