Understanding structure–activity relationships: iron(ii) complexes of “Legacy Guanidines” as catalysts for the synthesis of polylactide
Conrads, Christian; Burkart, Lisa; Soerensen, Sven; Noichl, Sandra; Kara, Yasemin; Heck, Joshua; Hoffmann, Alexander; Herres-Pawlis, Sonja; Catalysis Science & Technology 13 (2023) 6006–6021; doi:10.1039/D3CY01117H

data_1569889
_publ_section_title
;
 Understanding structure--activity relationships: iron(ii) complexes of
 &#x201C;Legacy Guanidines&#x201D; as catalysts for the synthesis of
 polylactide
;
_journal_issue                   20
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6006
_journal_page_last               6021
_journal_paper_doi               10.1039/D3CY01117H
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C13 H30 Cl2 Fe N6'
_chemical_formula_sum            'C13 H30 Cl2 Fe N6'
_chemical_formula_weight         397.18
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-02 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                69.47(3)
_cell_angle_beta                 87.94(3)
_cell_angle_gamma                65.38(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3007(19)
_cell_length_b                   9.830(2)
_cell_length_c                   12.490(3)
_cell_measurement_reflns_used    27644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.48
_cell_measurement_theta_min      2.43
_cell_volume                     964.0(5)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details      ' 2449 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23563
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.575
_diffrn_reflns_theta_min         2.429
_diffrn_source                   'Genix Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  0.8883
_exptl_absorpt_correction_T_min  0.3267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         7566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5772
_reflns_number_total             7566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy01117h2.cif
_cod_data_source_block           C4
_cod_depositor_comments
'Adding full bibliography for 1569886--1569893.cif.'
_cod_original_cell_volume        964.0(4)
_cod_database_code               1569889
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.892
_shelx_res_checksum              10897