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_7241135
_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 Fe N5, C F3 O3 S, C H4 O'
_chemical_formula_sum            'C14 H21 Cl2 F3 Fe N5 O4 S'
_chemical_formula_weight         539.17
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-21
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.928(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1639(3)
_cell_length_b                   8.8011(3)
_cell_length_c                   12.5028(4)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    99.97
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.89
_cell_volume                     1051.45(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      99.97
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37464
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.726
_diffrn_reflns_theta_min         2.891
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.0975 before and 0.0833 after correction. The Ratio of minimum to maximum transmission is 0.8699. 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    1.703
_exptl_crystal_description       prism
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0210P)^2^+4.1840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1861
_reflns_number_total             2152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra05756h2.cif
_cod_data_source_block           mm_i_110518_0m
_cod_depositor_comments
'Adding full bibliography for 7241133--7241138.cif.'
_cod_database_code               7241135
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: O1(0.5) H1(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
3.a Ternary CH refined with riding coordinates:
 N007(H007), N009(H009)
3.b Secondary CH2 refined with riding coordinates:
 C00E(H00A,H00B), C00H(H00C,H00D), C00I(H00E,H00F)
3.c Aromatic/amide H refined with riding coordinates:
 C00G(H00G)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
3.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'