Synthesis and characterization of α-diamine palladium complexes and insight into hybridization effects of nitrogen donor atoms on norbornene (co)polymerizations
Zheng, Ting; Liao, Heng; Gao, Jie; Zhong, Liu; Gao, Haiyang; Wu, Qing; Polymer Chemistry 9 (2018) 3088–; doi:10.1039/C8PY00395E

data_1549380
_publ_section_title
;
 Synthesis and characterization of \a-diamine palladium complexes and
 insight into hybridization effects of nitrogen donor atoms on norbornene
 (co)polymerizations
;
_journal_issue                   22
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3088
_journal_paper_doi               10.1039/C8PY00395E
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C28 H28 Cl2 N2 Pd, H2 O'
_chemical_formula_sum            'C28 H30 Cl2 N2 O Pd'
_chemical_formula_weight         587.84
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-03-09 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.678(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0031(4)
_cell_length_b                   17.0473(4)
_cell_length_c                   21.8047(7)
_cell_measurement_reflns_used    10218
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.0660
_cell_measurement_theta_min      3.6970
_cell_volume                     5078.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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    -17.00  60.00   1.00    3.00    --  -18.80   0.00 -60.00   77
  2  \w    -40.00  53.00   1.00    3.00    --  -18.80  57.00  30.00   93
  3  \w    -79.00 -42.00   1.00    3.00    --  -18.80   0.00 -60.00   37
  4  \w    -98.00 -65.00   1.00    3.00    --  -18.80 178.00-180.00   33
  5  \w    -92.00 -65.00   1.00    3.00    --  -18.80 178.00  90.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0212480000
_diffrn_orient_matrix_UB_12      0.0037017000
_diffrn_orient_matrix_UB_13      -0.0265473000
_diffrn_orient_matrix_UB_21      -0.0265018000
_diffrn_orient_matrix_UB_22      0.0352558000
_diffrn_orient_matrix_UB_23      -0.0085252000
_diffrn_orient_matrix_UB_31      0.0392645000
_diffrn_orient_matrix_UB_32      0.0217755000
_diffrn_orient_matrix_UB_33      0.0182909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28792
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.389
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.538
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         10370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0283P)^2^+2.0128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8624
_reflns_number_total             10370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py00395e2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1549377--1549380.cif.'
_cod_database_code               1549380
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Pd Cl'
_chemical_oxdiff_usercomment     anp-dmp
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O2(H2B,H2C), O1(H1B,H1C)
2.b Ternary CH refined with riding coordinates:
 N2(H2), N3(H3), N4(H4A), N1(H1), C29(H29), C2(H2A), C1(H1A), C30(H30)
2.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C9(H9), C7(H7), C32(H32), C37(H37), C33(H33), C8(H8), C35(H35),
 C36(H36), C6(H6), C4(H4), C43(H43), C51(H51), C25(H25), C23(H23), C15(H15),
 C45(H45), C5(H5), C44(H44), C53(H53), C17(H17), C24(H24), C16(H16), C52(H52)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C55(H55A,H55B,H55C), C19(H19A,H19B,H19C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C28(H28A,H28B,H28C), C56(H56A,H56B,H56C), C20(H20A,
 H20B,H20C)
;
_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 1.195
_oxdiff_exptl_absorpt_empirical_full_min 0.841