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_7247505
_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_absolute_configuration na
_chemical_formula_moiety         'C38 H47 Cl2 Fe N2 P'
_chemical_formula_sum            'C38 H46 Cl2 Fe N2 P'
_chemical_formula_weight         688.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 108.9370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.48430(10)
_cell_length_b                   12.94410(10)
_cell_length_c                   14.17160(10)
_cell_measurement_reflns_used    22745
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      76.7940
_cell_measurement_theta_min      3.2740
_cell_volume                     1819.13(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      170.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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     36.00 118.00   0.50    0.05    --   47.70  38.00   0.00  164
  2  \w     50.00  76.00   0.50    0.05    --   47.70  57.00 -60.00   52
  3  \w     33.00 112.00   0.50    0.05    --   47.70  57.00 -90.00  158
  4  \w     52.00  90.00   0.50    0.05    --   47.70  51.00-179.00   76
  5  \w     35.00  60.00   0.50    0.05    --  107.36 -57.00-180.00   50
  6  \w     35.00  64.00   0.50    0.05    --  107.36 -57.00 -90.00   58
  7  \w     -6.00  19.00   0.50    0.05    --   47.70 -51.00  34.00   50
  8  \w     37.00  68.00   0.50    0.05    --  107.36 -57.00 150.00   62
  9  \w     36.00  67.00   0.50    0.05    --  107.36 -57.00  30.00   62
 10  \w     36.00  61.00   0.50    0.05    --  107.36 -51.00  34.00   50
 11  \w    103.00 178.00   0.50    0.05    --  107.36  38.00 -30.00  150
 12  \w    150.00 176.00   0.50    0.05    --  107.36  77.00 -90.00   52
 13  \w     94.00 140.00   0.50    0.05    --  107.36  57.00 -60.00   92
 14  \w     94.00 133.00   0.50    0.05    --  107.36  51.00-179.00   78
 15  \w    152.00 178.00   0.50    0.05    --  107.36  51.00-179.00   52
 16  \w     86.00 131.00   0.50    0.05    --  107.36  77.00-120.00   90
 17  \w     85.00 111.00   0.50    0.05    --  107.36  77.00 -90.00   52
 18  \w    -20.00  28.00   0.50    0.05    --  -47.70  19.00 -30.00   96
 19  \w    -50.00  24.00   0.50    0.05    --  -47.70  51.00-179.00  148
 20  \w    -99.00 -74.00   0.50    0.05    -- -104.50  77.00-120.00   50
 21  \w    -99.00 -42.00   0.50    0.05    -- -104.50  77.00 -60.00  114
 22  \w    -62.00 -37.00   0.50    0.05    -- -104.50  57.00  60.00   50
 23  \w    -62.00 -32.00   0.50    0.05    -- -104.50  57.00   0.00   60
 24  \w    -59.00 -32.00   0.50    0.05    -- -104.50  57.00  30.00   54
 25  \w    -59.00 -33.00   0.50    0.05    -- -104.50  57.00 -60.00   52
 26  \w    -62.00 -36.00   0.50    0.05    -- -104.50  57.00 -90.00   52
 27  \w    -67.00 -41.00   0.50    0.05    -- -104.50  77.00-120.00   52
 28  \w     35.00 111.00   0.50    0.05    --  107.36-125.00-150.00  152
 29  \w   -109.00 -83.00   0.50    0.05    -- -104.50 -79.00 -29.92   52
 30  \w   -109.00 -83.00   0.50    0.05    -- -104.50 -77.00 -41.03   52
 31  \w   -172.00-119.00   0.50    0.05    -- -104.50 -77.00 -41.03  106
 32  \w   -171.00-145.00   0.50    0.05    -- -104.50 -77.00 -30.00   52
 33  \w   -160.00-134.00   0.50    0.05    -- -104.50 -77.00 -60.00   52
 34  \w   -113.00 -87.00   0.50    0.05    -- -104.50 -64.00 -69.65   52
 35  \w   -111.00 -85.00   0.50    0.05    -- -104.50 -77.00 -60.00   52
 36  \w   -173.00 -92.00   0.50    0.05    -- -104.50 -63.00-101.11  162
 37  \w   -173.00-118.00   0.50    0.05    -- -104.50 -69.00 -14.16  110
 38  \w   -113.00 -87.00   0.50    0.05    -- -104.50 -63.00 -94.36   52
 39  \w   -107.00 -82.00   0.50    0.05    -- -104.50 -77.00 -30.00   50
 40  \w   -115.00 -89.00   0.50    0.05    -- -104.50 -57.00 -60.00   52
 41  \w   -111.00 -85.00   0.50    0.05    -- -104.50 -69.00 -14.16   52
 42  \w   -115.00 -89.00   0.50    0.05    -- -104.50 -57.00 -90.00   52
 43  \w   -122.00 -90.00   0.50    0.05    -- -104.50 -57.00   0.00   64
 44  \w   -136.00-106.00   0.50    0.05    -- -104.50 -51.00  34.00   60
 45  \w   -172.00-136.00   0.50    0.05    -- -104.50 -57.00   0.00   72
 46  \w   -116.00 -90.00   0.50    0.05    -- -104.50 -48.00 -78.94   52
 47  \w   -117.00 -91.00   0.50    0.05    -- -104.50 -49.00 -85.25   52
 48  \w   -146.00 -93.00   0.50    0.05    -- -104.50 -41.00-102.53  106
 49  \w   -109.00 -71.00   0.50    0.05    --  -47.70 -51.00  34.00   76
 50  \w   -169.00 -87.00   0.50    0.05    -- -104.50 -64.00 135.27  164
 51  \w   -167.00 -90.00   0.50    0.05    -- -104.50 -58.00 114.28  154
 52  \w   -173.00 -91.00   0.50    0.05    -- -104.50 -38.00  60.00  164
 53  \w   -117.00 -91.00   0.50    0.05    -- -104.50 -38.00 -60.00   52
 54  \w   -120.00 -92.00   0.50    0.05    -- -104.50 -19.00-180.00   56
 55  \w   -118.00 -74.00   0.50    0.05    --  -47.70-125.00-180.00   88
 56  \w   -120.00 -91.00   0.50    0.05    --  -47.70-125.00 -90.00   58
 57  \w   -117.00 -79.00   0.50    0.05    --  -47.70-125.00 -60.00   76
 58  \w   -120.00 -75.00   0.50    0.05    --  -47.70-125.00  30.00   90
;
_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      0.1360583000
_diffrn_orient_matrix_UB_12      0.0216000000
_diffrn_orient_matrix_UB_13      0.0812860000
_diffrn_orient_matrix_UB_21      0.0714313000
_diffrn_orient_matrix_UB_22      -0.0708544000
_diffrn_orient_matrix_UB_23      -0.0544962000
_diffrn_orient_matrix_UB_31      0.0227990000
_diffrn_orient_matrix_UB_32      0.0930828000
_diffrn_orient_matrix_UB_33      -0.0603370000
_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  0.0294
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28114
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.041
_diffrn_reflns_theta_min         3.297
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46633
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.308(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0948P)^2^+4.0032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                7259
_reflns_number_total             7360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra05867k2.cif
_cod_data_source_block           Fe6
_cod_database_code               7247505
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Fe Cl'
_reflns_odcompleteness_completeness 99.94
_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), C30(H30), C33(H33), C36(H36)
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), C26(H26), C28(H28)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              85364
_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 1.883
_oxdiff_exptl_absorpt_empirical_full_min 0.614