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_7704351
_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         'C58 H65.96 Br0.04 N2 O2 P2, 0.96(C5 H12)'
_chemical_formula_sum            'C62.79 H77.45 Br0.04 N2 O2 P2'
_chemical_formula_weight         957.33
_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     dual
_audit_creation_date             2019-11-05
_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                73.03
_cell_angle_beta                 82.93
_cell_angle_gamma                88.87
_cell_formula_units_Z            2
_cell_length_a                   9.628
_cell_length_b                   15.392
_cell_length_c                   19.387
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.69
_cell_measurement_theta_min      2.41
_cell_volume                     2726.650
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Cu'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'QUAZAR MX multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25461
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.781
_diffrn_reflns_theta_max         66.781
_diffrn_reflns_theta_min         2.401
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'high brilliance microfocus sealed tube, Cu'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0873 before and 0.0563 after correction. The Ratio of minimum to maximum transmission is 0.8661. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       needle
_exptl_crystal_F_000             1031
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.970
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         9579
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0635P)^2^+3.6206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7729
_reflns_number_total             9579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00972e2.cif
_cod_data_source_block           1bH2
_cod_depositor_comments
'Adding full bibliography for 7704346--7704354.cif.'
_cod_original_cell_volume        2726.5
_cod_database_code               7704351
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.688
_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, All O(H) groups
2. Restrained distances
 C63-C62
 1.471 with sigma of 0.02
 C60-C59
 1.471 with sigma of 0.02
 C62-C61
 1.457 with sigma of 0.02
 C61-C60
 1.457 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C63, C62, C61, C60, C59} sigma for 1-2: 0.02, 1-3: 0.04
as
{C59, C60, C61, C62, C63}
5. Others
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(1)
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=FVAR(1)
 Sof(Br)=1-FVAR(2)
 Sof(H5)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=
 Sof(H63B)=Sof(H63C)=FVAR(2)
 Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(3)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C36(H36), C38(H38), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C18B(H18D,H18E,H18F), C19(H19A,H19B,H19C), C19B(H19D,H19E,H19F),
 C20(H20A,H20B,H20C), C20B(H20D,H20E,H20F), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C44B(H44D,H44E,H44F),
 C45(H45A,H45B,H45C), C45B(H45D,H45E,H45F), C46(H46A,H46B,H46C), C46B(H46D,H46E,
 H46F), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_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'