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_7247508
_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         'C23 H24 Cl Fe0.5 N2 O P, Cl4 Fe'
_chemical_formula_sum            'C23 H24 Cl5 Fe1.5 N2 O P'
_chemical_formula_weight         636.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-07
_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                 94.627(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0592(3)
_cell_length_b                   15.9546(4)
_cell_length_c                   13.9879(3)
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      74.8660
_cell_measurement_theta_min      4.1920
_cell_volume                     2682.50(11)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_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 0.956
_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     94.00 120.00   0.50    1.30    --  107.36  57.00   0.00   52
  2  \w    109.00 135.00   0.50    1.30    --  107.36 121.00  90.00   52
  3  \w    148.00 176.00   0.50    1.30    --  107.36  57.00   0.00   56
  4  \w     67.00  92.00   0.50    0.16    --   47.70 152.00-109.00   50
  5  \w     98.00 160.00   0.50    1.30    --  107.36  37.00-180.00  124
  6  \w     38.00  69.00   0.50    1.30    --  107.36 -57.00 -30.00   62
  7  \w     40.00  67.00   0.50    1.30    --  107.36 -57.00  30.00   54
  8  \w     79.00 104.00   0.50    1.30    --  107.36 -77.00  30.00   50
  9  \w     36.00 104.00   0.50    1.30    --  107.36-121.00   7.00  136
 10  \w     44.00 111.00   0.50    0.16    --   47.70-152.00-152.00  134
 11  \w     37.00 131.00   0.50    1.30    --  107.36-152.00-152.00  188
 12  \w     46.00  72.00   0.50    1.30    --  107.36 -99.00-150.00   52
 13  \w     55.00  80.00   0.50    0.16    --   47.70-121.00   7.00   50
 14  \w    -22.00  16.00   0.50    0.16    --  -47.70  19.00-150.00   76
 15  \w    -22.00  27.00   0.50    0.16    --  -47.70  19.00 -60.00   98
 16  \w    -22.00  27.00   0.50    0.16    --  -47.70  19.00  60.00   98
 17  \w    -58.00 -32.00   0.50    1.30    -- -104.50 125.00  30.00   52
 18  \w    -65.00 -32.00   0.50    1.30    -- -104.50 133.00  -5.77   66
 19  \w   -105.00 -80.00   0.50    1.30    -- -104.50 152.00-109.00   50
 20  \w   -117.00 -80.00   0.50    1.30    -- -104.50 133.00  -5.77   74
 21  \w   -100.00 -68.00   0.50    1.30    -- -104.50 125.00  30.00   64
 22  \w    -76.00 -51.00   0.50    0.16    --  -47.70 121.00  90.00   50
 23  \w    -95.00 -70.00   0.50    1.30    -- -104.50 121.00  90.00   50
 24  \w   -102.00 -35.00   0.50    1.30    -- -104.50  77.00  90.00  134
 25  \w    -62.00 -36.00   0.50    1.30    -- -104.50  57.00 120.00   52
 26  \w    -62.00 -36.00   0.50    1.30    -- -104.50  57.00  30.00   52
 27  \w    -62.00 -34.00   0.50    1.30    -- -104.50  57.00 -90.00   56
 28  \w    -63.00 -37.00   0.50    0.16    --  -47.70 -37.00 -90.00   52
 29  \w   -121.00 -75.00   0.50    0.16    --  -47.70 -37.00 -90.00   92
 30  \w   -167.00 -92.00   0.50    1.30    -- -104.50 -37.00   0.00  150
 31  \w   -119.00 -79.00   0.50    0.16    --  -47.70-125.00  60.00   80
 32  \w   -149.00-124.00   0.50    1.30    -- -104.50-121.00   7.00   50
 33  \w   -119.00 -67.00   0.50    0.16    --  -47.70-152.00-152.00  104
;
_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      -0.0718466000
_diffrn_orient_matrix_UB_12      0.0635250000
_diffrn_orient_matrix_UB_13      0.0504285000
_diffrn_orient_matrix_UB_21      0.0501803000
_diffrn_orient_matrix_UB_22      0.0720237000
_diffrn_orient_matrix_UB_23      -0.0558305000
_diffrn_orient_matrix_UB_31      -0.0934199000
_diffrn_orient_matrix_UB_32      -0.0101864000
_diffrn_orient_matrix_UB_33      -0.0809943000
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22038
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.419
_diffrn_reflns_theta_min         4.211
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29334
_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    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0537
_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^)+(0.1051P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4542
_reflns_number_total             5463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra05867k2.cif
_cod_data_source_block           Fe4'
_cod_original_formula_sum        'C23 H24 Cl5 Fe1.50 N2 O P'
_cod_database_code               7247508
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Fe Cl'
_reflns_odcompleteness_completeness 99.98
_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
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)
;
_shelx_res_checksum              94305
_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 2.435
_oxdiff_exptl_absorpt_empirical_full_min 0.562