Phosphasalen group IV metal complexes: synthesis, characterization and ring opening polymerization of lactide.
Normand, Adrien T.; Malacea-Kabbara, Raluca; Lapenta, Rosita; Dajnak, Aymeric; Richard, Philippe; Cattey, Hélène; Bolley, Anaëlle; Grassi, Alfonso; Milione, Stefano; Auffrant, Audrey; Dagorne, Samuel; Le Gendre, Pierre; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6989–7004; doi:10.1039/d0dt00972e

data_7704349
_publ_section_title
;
 Phosphasalen group IV metal complexes: synthesis, characterization and
 ring opening polymerization of lactide.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6989
_journal_page_last               7004
_journal_paper_doi               10.1039/d0dt00972e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C54 H66 N2 O2 P2, 0.1(C H2 Cl2)'
_chemical_formula_sum            'C54.1 H66.2 Cl0.2 N2 O2 P2'
_chemical_formula_weight         845.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.866(18)
_cell_length_b                   13.874(14)
_cell_length_c                   20.49(2)
_cell_measurement_reflns_used    5065
_cell_measurement_temperature    110
_cell_measurement_theta_max      26.096
_cell_measurement_theta_min      2.72
_cell_volume                     4790(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28200
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.990
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7785
_exptl_absorpt_correction_T_min  0.7092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0819 before and 0.0672 after correction. The Ratio of minimum to maximum transmission is 0.9110. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             1817
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0502P)^2^+2.1582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2606
_reflns_number_total             4189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00972e2.cif
_cod_data_source_block           1aH2
_cod_depositor_comments
'Adding full bibliography for 7704346--7704354.cif.'
_cod_original_cell_volume        4790(9)
_cod_original_formula_sum        'C54.10 H66.20 Cl0.20 N2 O2 P2'
_cod_database_code               7704349
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.986
_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. Uiso/Uaniso restraints and constraints
Uiso(Cl1) = Uiso(Cl2)
3. Rigid body (RIGU) restrains
 Cl2, C28, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Cl1(0.05) C28(0.05) H28A(0.05) H28B(0.05) Cl2(0.05)
5.a Riding coordinates:
 N(H)
5.b Free rotating group:
 Cl1(C28,Cl2)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C28(H28A,H28B)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27)
5.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'