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_7241138
_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         'C11 H17 Cl3 Fe N4, C F3 O3 S'
_chemical_formula_sum            'C12 H17 Cl3 F3 Fe N4 O3 S'
_chemical_formula_weight         516.558
_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     iterative
_audit_creation_date             2020-07-28
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-07-28 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.673(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9779(4)
_cell_length_b                   10.3829(6)
_cell_length_c                   13.9933(8)
_cell_measurement_reflns_used    9576
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      2.95
_cell_volume                     1004.75(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.3-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.9855
_diffrn_measured_fraction_theta_max 0.9884
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.9855
_diffrn_reflns_Laue_measured_fraction_max 0.9884
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            83932
_diffrn_reflns_point_group_measured_fraction_full 0.9855
_diffrn_reflns_point_group_measured_fraction_max 0.9884
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  .917
_exptl_absorpt_correction_T_min  .316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0530 before and 0.0416 after correction. The Ratio of minimum to maximum transmission is 1.0301. The \l/2 correction factor is Not present.'
_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    1.707
_exptl_crystal_description       prism
_exptl_crystal_F_000             524.113
_exptl_crystal_size_max          0.958
_exptl_crystal_size_mid          0.764
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.4243
_refine_diff_density_min         -0.3881
_refine_diff_density_rms         0.0650
_refine_ls_d_res_high            0.7166
_refine_ls_d_res_low             6.9154
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0497
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0497
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.9282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0613
_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              19
_reflns_limit_l_min              0
_reflns_number_gt                2898
_reflns_number_total             2977
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ra05756h2.cif
_cod_data_source_block           MM_II_061419_FeL8_0m
_cod_depositor_comments
'Adding full bibliography for 7241133--7241138.cif.'
_cod_database_code               7241138
_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), N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C2(H2a,H2b)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'