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_7704350
_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         'C59 H78 N4 O2 P2 Ti'
_chemical_formula_sum            'C59 H78 N4 O2 P2 Ti'
_chemical_formula_weight         985.09
_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             2020-01-14
_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                 97.910(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.449(3)
_cell_length_b                   27.820(7)
_cell_length_c                   14.860(4)
_cell_measurement_reflns_used    7564
_cell_measurement_temperature    115
_cell_measurement_theta_max      23.85
_cell_measurement_theta_min      2.20
_cell_volume                     5507(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      115.0
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            67556
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.657
_diffrn_reflns_theta_min         2.596
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0680 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.8954. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of benzene and pentane  by slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         12796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0342P)^2^+4.7140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8710
_reflns_number_total             12796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00972e2.cif
_cod_data_source_block           6c
_cod_depositor_comments
'Adding full bibliography for 7704346--7704354.cif.'
_cod_database_code               7704350
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C41B)=Sof(H41d)=Sof(H41e)=Sof(H41f)=Sof(C42B)=Sof(H42d)=Sof(H42e)=
 Sof(H42f)=Sof(C43B)=Sof(H43d)=Sof(H43e)=Sof(H43f)=1-FVAR(1)
 Sof(C41)=Sof(H41a)=Sof(H41b)=Sof(H41c)=Sof(C42)=Sof(H42a)=Sof(H42b)=Sof(H42c)=
 Sof(C43)=Sof(H43a)=Sof(H43b)=Sof(H43c)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
4.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C15(H15a,H15b,
 H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C37(H37a,H37b,H37c), C38(H38a,
 H38b,H38c), C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C41B(H41d,H41e,H41f),
 C42(H42a,H42b,H42c), C42B(H42d,H42e,H42f), C43(H43a,H43b,H43c), C43B(H43d,H43e,
 H43f), C56(H56a,H56b,H56c), C57(H57a,H57b,H57c), C58(H58a,H58b,H58c), C59(H59a,
 H59b,H59c)
;
_shelx_res_checksum              52268
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'