N-(2-(Diphenylphosphino)ethyl)-2-alkyl-5,6,7,8-tetrahydro-quinolin-8-amines iron(ii) complexes: structural diversity and the ring opening polymerization of ε-caprolactone
Wang, Yun; Zhang, Wenjuan; Wang, Xing; Zuo, Weiwei; Xue, Xiaopan; Ma, Yanping; Sun, Wen-Hua; RSC Advances 13 (2023) 29866–29878; doi:10.1039/D3RA05867K

data_7247509
_publ_section_title
;
 N-(2-(Diphenylphosphino)ethyl)-2-alkyl-5,6,7,8-tetrahydro-quinolin-8-amines
 iron(ii) complexes: structural diversity and the ring opening
 polymerization of \e-caprolactone
;
_journal_issue                   43
_journal_name_full               'RSC Advances'
_journal_page_first              29866
_journal_page_last               29878
_journal_paper_doi               10.1039/D3RA05867K
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C24 H27 Cl2 Fe N2 P'
_chemical_formula_sum            'C24 H26 Cl2 Fe N2 P'
_chemical_formula_weight         500.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-08-16 deposited with the CCDC.	2023-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.08330(10)
_cell_length_b                   15.72850(10)
_cell_length_c                   12.54790(10)
_cell_measurement_reflns_used    20749
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.8900
_cell_measurement_theta_min      3.7000
_cell_volume                     2348.81(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     33.00 115.00   0.50    0.05    --   47.70  57.00  30.00  164
  2  \w    143.00 169.00   0.50    0.15    --  107.36  57.00  90.00   52
  3  \w     94.00 122.00   0.50    0.15    --  107.36  57.00  90.00   56
  4  \w    120.00 177.00   0.50    0.15    --  107.36  57.00  60.00  114
  5  \w     93.00 175.00   0.50    0.15    --  107.36  57.00  30.00  164
  6  \w     93.00 118.00   0.50    0.15    --  107.36  57.00 -30.00   50
  7  \w     96.00 152.00   0.50    0.15    --  107.36  19.00 -90.00  112
  8  \w     97.00 171.00   0.50    0.15    --  107.36  19.00 -60.00  148
  9  \w     95.00 178.00   0.50    0.15    --  107.36  19.00 -30.00  166
 10  \w    145.00 177.00   0.50    0.15    --  107.36  57.00 -30.00   64
 11  \w    -20.00   6.00   0.50    0.05    --  -47.70  19.00   0.00   52
 12  \w    -23.00  10.00   0.50    0.05    --  -47.70  19.00 -30.00   66
 13  \w    -16.00  26.00   0.50    0.05    --  -47.70  19.00-120.00   84
 14  \w    149.00 175.00   0.50    0.15    --  107.36  81.00 -11.00   52
 15  \w    112.00 147.00   0.50    0.15    --  107.36  81.00 -11.00   70
 16  \w    -26.00  30.00   0.50    0.05    --   47.70 -19.00-120.00  112
 17  \w    -25.00  23.00   0.50    0.05    --   47.70 -19.00 -60.00   96
 18  \w    -22.00   4.00   0.50    0.05    --   47.70 -19.00  60.00   52
 19  \w     39.00  69.00   0.50    0.15    --  107.36 -57.00   0.00   60
 20  \w     36.00  68.00   0.50    0.15    --  107.36 -57.00  60.00   64
 21  \w     39.00  69.00   0.50    0.15    --  107.36 -57.00  90.00   60
 22  \w     35.00  67.00   0.50    0.15    --  107.36 -57.00 -60.00   64
 23  \w     35.00  69.00   0.50    0.15    --  107.36 -57.00 -90.00   68
 24  \w     38.00  68.00   0.50    0.15    --  107.36 -57.00-120.00   60
 25  \w     36.00  69.00   0.50    0.15    --  107.36 -57.00-150.00   66
 26  \w     39.00 106.00   0.50    0.15    --  107.36 -99.00-150.00  134
 27  \w     53.00 101.00   0.50    0.15    --  107.36 -81.00-133.00   96
 28  \w    -23.00  70.00   0.50    0.05    --   47.70 -81.00-133.00  186
 29  \w    -62.00 -33.00   0.50    0.15    -- -104.50 125.00 -30.00   58
 30  \w   -111.00 -66.00   0.50    0.15    -- -104.50 125.00 -30.00   90
 31  \w   -110.00 -61.00   0.50    0.15    -- -104.50 125.00 -60.00   98
 32  \w   -110.00 -56.00   0.50    0.15    -- -104.50 125.00 -90.00  108
 33  \w    -73.00 -47.00   0.50    0.15    -- -104.50  81.00 -11.00   52
 34  \w    -59.00  24.00   0.50    0.05    --  -47.70  81.00 -11.00  166
 35  \w    -59.00 -32.00   0.50    0.15    -- -104.50  57.00-120.00   54
 36  \w    -92.00 -41.00   0.50    0.15    -- -104.50  77.00-180.00  102
 37  \w    -62.00 -33.00   0.50    0.15    -- -104.50  57.00-180.00   58
 38  \w   -148.00-122.00   0.50    0.15    -- -104.50 -38.00-180.00   52
 39  \w   -172.00 -90.00   0.50    0.15    -- -104.50 -57.00-180.00  164
 40  \w   -117.00 -91.00   0.50    0.15    -- -104.50 -57.00 -90.00   52
 41  \w   -171.00-130.00   0.50    0.15    -- -104.50 -57.00 -90.00   82
 42  \w   -174.00 -92.00   0.50    0.15    -- -104.50 -19.00  90.00  164
 43  \w   -151.00 -93.00   0.50    0.15    -- -104.50 -19.00 120.00  116
 44  \w   -119.00 -75.00   0.50    0.05    --  -47.70-125.00  30.00   88
 45  \w   -173.00-131.00   0.50    0.15    -- -104.50 -81.00-133.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1178359000
_diffrn_orient_matrix_UB_12      -0.0255990000
_diffrn_orient_matrix_UB_13      -0.0198276000
_diffrn_orient_matrix_UB_21      0.0047557000
_diffrn_orient_matrix_UB_22      0.0806549000
_diffrn_orient_matrix_UB_23      -0.0687320000
_diffrn_orient_matrix_UB_31      0.0534286000
_diffrn_orient_matrix_UB_32      0.0492929000
_diffrn_orient_matrix_UB_33      0.1020823000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32335
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.361
_diffrn_reflns_theta_min         3.714
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.984
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+1.6999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4768
_reflns_number_total             4890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra05867k2.cif
_cod_data_source_block           Fe2
_cod_database_code               7247509
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Fe Cl'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Ternary CH refined with riding coordinates:
 N2(H2), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_shelx_res_checksum              48229
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.413
_oxdiff_exptl_absorpt_empirical_full_min 0.844