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_7247504
_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         'C46 H50 Cl4 Fe2 N4 P2'
_chemical_formula_sum            'C46 H50 Cl4 Fe2 N4 P2'
_chemical_formula_weight         974.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-17
_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                71.656(4)
_cell_angle_beta                 78.877(5)
_cell_angle_gamma                85.997(4)
_cell_formula_units_Z            1
_cell_length_a                   8.5815(5)
_cell_length_b                   10.7155(4)
_cell_length_c                   14.7219(8)
_cell_measurement_reflns_used    10669
_cell_measurement_temperature    169.98(11)
_cell_measurement_theta_max      75.2380
_cell_measurement_theta_min      3.1790
_cell_volume                     1260.76(12)
_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      169.98(11)
_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 0.968
_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     25.00 120.00   0.50    0.08    --   47.70  77.00  12.00  190
  2  \w     25.00 120.00   0.50    0.08    --   47.70  77.00 120.00  190
  3  \w     25.00 120.00   0.50    0.08    --   47.70  77.00 -90.00  190
  4  \w     33.00 102.00   0.50    0.08    --   47.70  57.00   0.00  138
  5  \w     35.00  69.00   0.50    0.50    --  107.36 -57.00 120.00   68
  6  \w     35.00  69.00   0.50    0.50    --  107.36 -57.00  30.00   68
  7  \w     35.00  69.00   0.50    0.50    --  107.36 -57.00   0.00   68
  8  \w     35.00 109.00   0.50    0.50    --  107.36 -77.00 -60.00  148
  9  \w     35.00 109.00   0.50    0.50    --  107.36 -77.00-113.00  148
 10  \w     35.00 106.00   0.50    0.50    --  107.36 -99.00 -90.00  142
 11  \w     35.00 106.00   0.50    0.50    --  107.36 -99.00-150.00  142
 12  \w     35.00 111.00   0.50    0.50    --  107.36-125.00-150.00  152
 13  \w     19.00  95.00   0.50    0.08    --   47.70-125.00   0.00  152
 14  \w     35.00 106.00   0.50    0.50    --  107.36 -99.00 120.00  142
 15  \w    -27.00  30.00   0.50    0.08    --   47.70 -19.00-120.00  114
 16  \w    -24.00  70.00   0.50    0.08    --   47.70 -77.00-113.00  188
 17  \w     85.00 178.00   0.50    0.50    --  107.36  77.00  12.00  186
 18  \w     94.00 178.00   0.50    0.50    --  107.36  38.00 120.00  168
 19  \w   -126.00 -32.00   0.50    0.50    -- -104.50 145.00 145.67  188
 20  \w   -123.00 -32.00   0.50    0.50    -- -104.50 141.00  81.36  182
 21  \w    -95.00 -13.00   0.50    0.08    --  -47.70 125.00  30.00  164
 22  \w   -111.00 -32.00   0.50    0.50    -- -104.50 125.00  60.00  158
 23  \w   -111.00 -32.00   0.50    0.50    -- -104.50 125.00  30.00  158
 24  \w   -111.00 -32.00   0.50    0.50    -- -104.50 125.00 -30.00  158
 25  \w   -111.00 -32.00   0.50    0.50    -- -104.50 125.00 -60.00  158
 26  \w   -122.00 -32.00   0.50    0.50    -- -104.50 139.00-117.00  180
 27  \w    -70.00  25.00   0.50    0.08    --  -47.70  77.00  12.00  190
 28  \w   -102.00 -32.00   0.50    0.50    -- -104.50  77.00  12.00  140
 29  \w    -62.00 -32.00   0.50    0.50    -- -104.50  57.00 -90.00   60
 30  \w    -62.00 -32.00   0.50    0.50    -- -104.50  57.00-180.00   60
 31  \w   -174.00 -92.00   0.50    0.50    -- -104.50 -19.00 -60.00  164
 32  \w   -174.00 -82.00   0.50    0.50    -- -104.50 -77.00-113.00  184
 33  \w   -174.00 -89.00   0.50    0.50    -- -104.50 -57.00-150.00  170
 34  \w   -174.00 -92.00   0.50    0.50    -- -104.50 -46.00 -75.60  164
 35  \w   -120.00 -25.00   0.50    0.08    --  -47.70 -77.00-113.00  190
 36  \w   -174.00 -90.00   0.50    0.50    -- -104.50 -54.00  99.45  168
 37  \w   -120.00 -74.00   0.50    0.08    --  -47.70-125.00  60.00   92
 38  \w   -174.00 -86.00   0.50    0.50    -- -104.50 -99.00   0.00  176
;
_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      -0.0760694000
_diffrn_orient_matrix_UB_12      -0.1338670000
_diffrn_orient_matrix_UB_13      0.0598433000
_diffrn_orient_matrix_UB_21      -0.1147046000
_diffrn_orient_matrix_UB_22      0.0195258000
_diffrn_orient_matrix_UB_23      -0.0720822000
_diffrn_orient_matrix_UB_31      0.1205535000
_diffrn_orient_matrix_UB_32      -0.0681366000
_diffrn_orient_matrix_UB_33      -0.0615373000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24265
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.175
_diffrn_reflns_theta_min         3.215
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68475
_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    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5177
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.1022
_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^)+(0.1124P)^2^+4.7278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2587
_refine_ls_wR_factor_ref         0.2686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4298
_reflns_number_total             5177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra05867k2.cif
_cod_data_source_block           Fe1
_cod_database_code               7247504
_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. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C20 \\sim C21 \\sim C23: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
3. Others
 Sof(C18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=Sof(C23)=Sof(H23)=1-FVAR(1)
 Sof(C24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(H28)=Sof(C29)=Sof(H29)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N2(H2), C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23)
;
_shelx_res_checksum              41278
_shelx_fab_checksum              98359
_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 2.236
_oxdiff_exptl_absorpt_empirical_full_min 0.713