Initiating abilities of diphosphine- and diamine-ligated Pd complexes/NaBPh4 systems for C1 polymerization of diazoacetates
Shimomoto, Hiroaki; Miyano, Yuto; Kinoshita, Kaito; Itoh, Tomomichi; Ihara, Eiji; Polymer Chemistry 14 (2023) 1007–1018; doi:10.1039/D2PY01548J

data_1568376
_publ_section_title
;
 Initiating abilities of diphosphine- and diamine-ligated Pd
 complexes/NaBPh4 systems for C1 polymerization of diazoacetates
;
_journal_issue                   9
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1007
_journal_page_last               1018
_journal_paper_doi               10.1039/D2PY01548J
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C46 H34 Cl2 O2 P2 Pd, 1.45(C3 H6 O)'
_chemical_formula_sum            'C50.34 H42.68 Cl2 O3.45 P2 Pd'
_chemical_formula_weight         942.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-20 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.985(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4623(3)
_cell_length_b                   10.8537(3)
_cell_length_c                   32.8318(8)
_cell_measurement_reflns_used    32664
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.2190
_cell_measurement_theta_min      1.9570
_cell_volume                     4430.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50    2.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    2.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50    2.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00  70.00   0.50    2.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0111707000
_diffrn_orient_matrix_UB_12      -0.0422069000
_diffrn_orient_matrix_UB_13      -0.0156524000
_diffrn_orient_matrix_UB_21      -0.0558170000
_diffrn_orient_matrix_UB_22      -0.0051023000
_diffrn_orient_matrix_UB_23      -0.0056079000
_diffrn_orient_matrix_UB_31      0.0037988000
_diffrn_orient_matrix_UB_32      0.0496408000
_diffrn_orient_matrix_UB_33      -0.0138741000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            73717
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.638
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1929
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10694
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0605P)^2^+7.8508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8162
_reflns_number_total             10694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01548j2.cif
_cod_data_source_block           shimomoto
_cod_depositor_comments
'Adding full bibliography for 1568372--1568378.cif.'
_cod_database_code               1568376
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H19 Cl2 O2 Pd1'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C49 \\sim C47 \\sim O3 \\sim C48: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C52 \\sim O4 \\sim C50 \\sim C51: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O3) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(O4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C49, C47, O3, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, C50, O4, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O3)=Sof(C47)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C48)=Sof(H48A)=
 Sof(H48B)=Sof(H48C)=FVAR(1)
 Sof(C50)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(O4)=Sof(C52)=Sof(H52A)=
 Sof(H52B)=Sof(H52C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C36(H36), C40(H40), C30(H30), C38(H38), C46(H46), C42(H42),
 C28(H28), C22(H22), C24(H24), C27(H27), C37(H37), C33(H33), C39(H39), C31(H31),
  C26(H26), C21(H21), C32(H32), C43(H43), C45(H45), C4(H4), C25(H25), C18(H18),
 C16(H16), C44(H44), C12(H12), C5(H5), C20(H20), C7(H7), C19(H19), C15(H15),
 C6(H6), C14(H14), C13(H13)
5.b Idealised Me refined with riding coordinates:
 C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C)
;
_shelx_res_checksum              46979
_olex2_exptl_crystal_mounting_method loops
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.253
_oxdiff_exptl_absorpt_empirical_full_min 0.703