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_7247507
_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 Cl3 Fe N2 P'
_chemical_formula_sum            'C23 H23 Cl3 Fe N2 P'
_chemical_formula_weight         520.60
_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             2021-12-13
_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                 115.527(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2884(3)
_cell_length_b                   19.7047(3)
_cell_length_c                   11.5379(3)
_cell_measurement_reflns_used    7652
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      75.0730
_cell_measurement_theta_min      4.4770
_cell_volume                     2315.90(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      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 0.964
_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    -22.00  67.00   0.50    0.05    --   47.68 -73.00  26.00  178
  2  \w     72.00 100.00   0.50    0.05    --   47.68  73.00 156.00   56
  3  \w     88.00 177.00   0.50    0.09    --  106.75  73.00 156.00  178
  4  \w     48.00  91.00   0.50    0.09    --  106.75 -73.00  26.00   86
  5  \w     34.00  60.00   0.50    0.09    --  106.75 -57.00 -60.00   52
  6  \w     37.00  63.00   0.50    0.09    --  106.75 -57.00-120.00   52
  7  \w     41.00  67.00   0.50    0.09    --  106.75 -57.00-150.00   52
  8  \w     34.00  65.00   0.50    0.09    --  106.75 -57.00-180.00   62
  9  \w     36.00  64.00   0.50    0.09    --  106.75 -57.00  60.00   56
 10  \w     41.00  68.00   0.50    0.09    --  106.75 -57.00 150.00   54
 11  \w     99.00 177.00   0.50    0.09    --  106.75  38.00 -90.00  156
 12  \w    -87.00 -37.00   0.50    0.09    -- -104.50  73.00 156.00  100
 13  \w   -101.00 -39.00   0.50    0.09    -- -104.50  77.00-120.00  124
 14  \w    -59.00 -32.00   0.50    0.09    -- -104.50  57.00  90.00   54
 15  \w    -66.00  18.00   0.50    0.05    --  -47.68  73.00 156.00  168
 16  \w    -62.00 -37.00   0.50    0.09    -- -104.50  57.00 120.00   50
 17  \w    -62.00 -37.00   0.50    0.09    -- -104.50  57.00 -30.00   50
 18  \w     38.00  76.00   0.50    0.09    --  106.75 -99.00   0.00   76
 19  \w    -58.00 -33.00   0.50    0.09    -- -104.50  57.00-150.00   50
 20  \w   -171.00 -94.00   0.50    0.09    -- -104.50 -38.00  90.00  154
 21  \w   -165.00-139.00   0.50    0.09    -- -104.50 -73.00  26.00   52
 22  \w   -119.00 -76.00   0.50    0.05    --  -47.68-125.00  90.00   86
 23  \w    -94.00 -69.00   0.50    0.05    --  -47.68 -73.00  26.00   50
 24  \w   -118.00 -74.00   0.50    0.05    --  -47.68-125.00-180.00   88
;
_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      0.1186984000
_diffrn_orient_matrix_UB_12      -0.0014054000
_diffrn_orient_matrix_UB_13      0.1327899000
_diffrn_orient_matrix_UB_21      -0.0535749000
_diffrn_orient_matrix_UB_22      0.0631149000
_diffrn_orient_matrix_UB_23      0.0404913000
_diffrn_orient_matrix_UB_31      -0.0769032000
_diffrn_orient_matrix_UB_32      -0.0461165000
_diffrn_orient_matrix_UB_33      0.0512565000
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16218
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.663
_diffrn_reflns_theta_min         4.488
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81729
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0401P)^2^+1.5580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4232
_reflns_number_total             4709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra05867k2.cif
_cod_data_source_block           Fe4
_cod_database_code               7247507
_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
2.a Ternary CH refined with riding coordinates:
 N2(H2), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C11(H11a,H11b), C7(H7a,H7b), C5(H5a,H5b), C6(H6a,H6b)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C20(H20), C23(H23), C22(H22), C2(H2a), C3(H3), C15(H15),
 C13(H13), C17(H17), C14(H14), C16(H16)
;
_shelx_res_checksum              20795
_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 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.858