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_1568378
_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
'C59 H42 Cl2 O3 P2 Pd, 0.5(C4 H8 O), 0.5(C4 H10 O)'
_chemical_formula_sum            'C63 H51 Cl2 O4 P2 Pd'
_chemical_formula_weight         1111.28
_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             2022-09-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-15 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.670(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2129(9)
_cell_length_b                   13.6540(4)
_cell_length_c                   20.7338(8)
_cell_measurement_reflns_used    30121
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.2720
_cell_measurement_theta_min      1.8130
_cell_volume                     5113.4(4)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    4.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    4.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50    4.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00  70.00   0.50    4.00    --  -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      0.0045681000
_diffrn_orient_matrix_UB_12      0.0185605000
_diffrn_orient_matrix_UB_13      0.0337218000
_diffrn_orient_matrix_UB_21      -0.0039599000
_diffrn_orient_matrix_UB_22      0.0484704000
_diffrn_orient_matrix_UB_23      -0.0135713000
_diffrn_orient_matrix_UB_31      -0.0387742000
_diffrn_orient_matrix_UB_32      -0.0026967000
_diffrn_orient_matrix_UB_33      -0.0120105000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            77041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.853
_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    0.581
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10598
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+1.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7775
_reflns_number_total             10598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01548j2.cif
_cod_data_source_block           miyanog17_autored
_cod_depositor_comments
'Adding full bibliography for 1568372--1568378.cif.'
_cod_database_code               1568378
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_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. Restrained distances
 O4-C60 = O4-C63
 1.44 with sigma of 0.02
 C60-C61 = C62-C63
 1.53 with sigma of 0.02
 C61-C62
 1.54 with sigma of 0.02
 O5-C1B
 1.41 with sigma of 0.02
 C1C-C1D
 1.5 with sigma of 0.02
 O5-C1C
 1.42 with sigma of 0.02
 C1A-C1B
 1.48 with sigma of 0.02
 O4-C61 = O4-C62 = C60-C62 = C61-C63
 2.38 with sigma of 0.04
 O5-C1A = O5-C1D
 2.37 with sigma of 0.04
 C61-C63 \\sim C60-C62
 with sigma of 0.04
 O4-C61 \\sim O4-C62
 with sigma of 0.04
 C60-C61 \\sim C61-C62 \\sim C62-C63
 with sigma of 0.02
 O4-C60 \\sim O4-C63
 with sigma of 0.02
 C1A-O5 \\sim O5-C1D
 with sigma of 0.04
 O5-C1B \\sim O5-C1C
 with sigma of 0.02
 C1A-C1B \\sim C1C-C1D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C60 \\sim C61 \\sim C62 \\sim C63: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O5 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O4, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O4(0.5) C60(0.5) H60A(0.5) H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5)
 C62(0.5) H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) O5(0.5) C1A(0.5)
 H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) C1C(0.5) H1CA(0.5)
 H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C1B(H1BA,
 H1BB), C1C(H1CA,H1CB)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17), C18(H18),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C43(H43), C44(H44),
 C45(H45), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59)
6.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,
 H1DC)
;
_shelx_res_checksum              97977
_olex2_exptl_crystal_mounting_method loop
_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 3.610
_oxdiff_exptl_absorpt_empirical_full_min 0.721