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_7704353
_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         'C64 H78 N2 O4 P2 Zr, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H82 Cl4 N2 O4 P2 Zr'
_chemical_formula_weight         1262.29
_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             2019-10-31
_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                104.471(3)
_cell_angle_beta                 102.628(3)
_cell_angle_gamma                101.728(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3206(9)
_cell_length_b                   13.3221(8)
_cell_length_c                   22.2555(13)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    115
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.61
_cell_volume                     3589.9(4)
_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      115
_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 0.994
_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  0.0822
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94359
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         2.130
_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    0.389
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0830 before and 0.0680 after correction. The Ratio of minimum to maximum transmission is 0.8625. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.845
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         16522
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+23.0599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2468
_refine_ls_wR_factor_ref         0.2619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12337
_reflns_number_total             16522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00972e2.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7704346--7704354.cif.'
_cod_database_code               7704353
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.909
_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 C(H,H,H,H,H,H) groups
2. Rigid body (RIGU) restrains
 C7, C7A, C8, C8A, C9, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C7(0.54691) H7(0.54691) C7A(0.45309) H7A(0.45309) C8(0.54691)
 H8A(0.54691) H8B(0.54691) H8C(0.54691) C8A(0.45309) H8AA(0.45309)
 H8AB(0.45309) H8AC(0.45309) C9(0.54691) H9A(0.54691) H9B(0.54691) H9C(0.54691)
 C9A(0.45309) H9AA(0.45309) H9AB(0.45309) H9AC(0.45309) C10(0.63664)
 H10(0.63664) C10A(0.36336) H10A(0.36336) H11A(0.63664) H11B(0.63664)
 H11C(0.63664) H11D(0.36336) H11E(0.36336) H11F(0.36336) H12A(0.63664)
 H12B(0.63664) H12C(0.63664) H12D(0.36336) H12E(0.36336) H12F(0.36336)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C7A(H7A), C10(H10), C10A(H10A)
4.b Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C66(H66A,H66B)
4.c Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C11(H11D,H11E,H11F), C12(H12A,H12B,H12C), C12(H12D,H12E,
 H12F)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C15(H15), C17(H17), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C41(H41), C43(H43), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
 C60(H60), C61(H61), C62(H62), C63(H63), C64(H64)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_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'