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_1568375
_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         'C49 H36 Cl2 O3 P2 Pd, 2(C4 H8 O)'
_chemical_formula_sum            'C57 H52 Cl2 O5 P2 Pd'
_chemical_formula_weight         1056.22
_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             2022-01-04
_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                67.524(4)
_cell_angle_beta                 81.219(4)
_cell_angle_gamma                78.077(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6300(5)
_cell_length_b                   13.0697(5)
_cell_length_c                   16.0599(6)
_cell_measurement_reflns_used    27013
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.1480
_cell_measurement_theta_min      1.8520
_cell_volume                     2388.82(18)
_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      100.0
_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 0.995
_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    1.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_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      -0.0211269000
_diffrn_orient_matrix_UB_12      -0.0265065000
_diffrn_orient_matrix_UB_13      -0.0235289000
_diffrn_orient_matrix_UB_21      -0.0527979000
_diffrn_orient_matrix_UB_22      0.0122170000
_diffrn_orient_matrix_UB_23      0.0199970000
_diffrn_orient_matrix_UB_31      -0.0090929000
_diffrn_orient_matrix_UB_32      0.0518734000
_diffrn_orient_matrix_UB_33      -0.0366892000
_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  0.0787
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42039
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         1.653
_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    0.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (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    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         12635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0389P)^2^+0.7741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10367
_reflns_number_total             12635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01548j2.cif
_cod_data_source_block           miyanoe16
_cod_depositor_comments
'Adding full bibliography for 1568372--1568378.cif.'
_cod_database_code               1568375
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C49H36Cl2O3P2Pd
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.908
_reflns_odcompleteness_completeness 89.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.016) H46(0.021) H14A(0.025) H14B(0.025) H14C(0.025)
 H21(0.017) H24(0.022) H4(0.015) H3(0.017) H23(0.017) H8(0.015) H9(0.017)
 H27(0.017) H10(0.015) H25(0.024) H36(0.024) H20(0.022) H15A(0.024) H15B(0.024)
 H15C(0.024) H30(0.021) H35(0.023) H34(0.017) H29(0.023) H18(0.022) H28(0.018)
 H26(0.023) H43(0.022) H37(0.025) H17(0.018) H32(0.019) H45(0.027) H38(0.019)
 H19(0.024) H44(0.029) H31(0.022) H50A(0.031) H50B(0.031) H53A(0.031)
 H53B(0.031) H55A(0.036) H55B(0.036) H52A(0.031) H52B(0.031) H54A(0.032)
 H54B(0.032) H51A(0.032) H51B(0.032) H57A(0.039) H57B(0.039) H56A(0.051)
 H56B(0.051)
 Fixed X: H2(1.077843) H46(0.470704) H14A(1.056889) H14B(0.991269)
 H14C(1.086279) H21(0.964651) H24(0.581645) H4(1.131628) H3(1.186145)
 H23(0.712922) H8(0.934237) H9(0.830132) H27(0.836168) H10(0.731513)
 H25(0.576398) H36(0.271205) H20(1.093321) H15A(0.879389) H15B(0.797023)
 H15C(0.815555) H30(0.736885) H35(0.324041) H34(0.509081) H29(0.848658)
 H18(1.126042) H28(0.835863) H26(0.705799) H43(0.268237) H37(0.40005)
 H17(0.997742) H32(0.599904) H45(0.290119) H38(0.58482) H19(1.176737)
 H44(0.189732) H31(0.613408) H50A(0.813066) H50B(0.700013) H53A(0.919785)
 H53B(0.964962) H55A(0.372351) H55B(0.308041) H52A(0.88048) H52B(0.979914)
 H54A(0.426307) H54B(0.421278) H51A(0.866103) H51B(0.769855) H57A(0.620138)
 H57B(0.592831) H56A(0.444156) H56B(0.444568)
 Fixed Y: H2(0.54907) H46(0.527597) H14A(0.193095) H14B(0.210312)
 H14C(0.28129) H21(0.666131) H24(0.755395) H4(0.291797) H3(0.38603)
 H23(0.80442) H8(0.347969) H9(0.480372) H27(0.474222) H10(0.644416)
 H25(0.565962) H36(0.718894) H20(0.746786) H15A(0.231276) H15B(0.34511)
 H15C(0.249331) H30(1.082181) H35(0.892659) H34(0.904611) H29(1.064109)
 H18(0.951595) H28(0.924615) H26(0.425587) H43(0.885517) H37(0.55527)
 H17(0.871118) H32(0.8169) H45(0.54668) H38(0.565735) H19(0.88702)
 H44(0.724227) H31(0.957306) H50A(0.823459) H50B(0.90848) H53A(0.997357)
 H53B(0.889447) H55A(0.645121) H55B(0.756054) H52A(1.111291) H52B(1.02522)
 H54A(0.60672) H54B(0.737245) H51A(0.951147) H51B(1.048082) H57A(0.774868)
 H57B(0.66393) H56A(0.861425) H56B(0.78589)
 Fixed Z: H2(0.073229) H46(0.210247) H14A(0.444662) H14B(0.533063)
 H14C(0.480907) H21(-0.067219) H24(-0.077795) H4(0.31153) H3(0.159771) H23(-
 0.017708) H8(0.586062) H9(0.643631) H27(0.102634) H10(0.547975) H25(-0.047112)
 H36(0.385599) H20(-0.182059) H15A(0.376365) H15B(0.36766) H15C(0.465029)
 H30(0.484437) H35(0.35019) H34(0.339117) H29(0.359421) H18(-0.054617)
 H28(0.30524) H26(0.041215) H43(0.079471) H37(0.418688) H17(0.061536)
 H32(0.505427) H45(0.181724) H38(0.414543) H19(-0.174768) H44(0.115684)
 H31(0.559091) H50A(0.806847) H50B(0.787637) H53A(0.588526) H53B(0.672849)
 H55A(0.780736) H55B(0.709098) H52A(0.671583) H52B(0.72567) H54A(0.652086)
 H54B(0.589482) H51A(0.846739) H51B(0.797632) H57A(0.694646) H57B(0.777743)
 H56A(0.692535) H56B(0.798933)
;
_shelx_res_checksum              6259
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.188
_oxdiff_exptl_absorpt_empirical_full_min 0.770