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_1549379
_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         'C36 H44 Cl2 N2 Pd, H2 O'
_chemical_formula_sum            'C36 H46 Cl2 N2 O Pd'
_chemical_formula_weight         700.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-03-05 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.56450(10)
_cell_length_b                   21.3415(3)
_cell_length_c                   13.8095(2)
_cell_measurement_reflns_used    14718
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.3050
_cell_measurement_theta_min      3.8000
_cell_volume                     3408.24(7)
_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 21.1652
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_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    -84.00  14.00   1.00   70.34    --  -10.40 -57.00-180.00   98
  2  \w    -36.00  55.00   1.00   70.34    --  -10.40  57.00 -30.00   91
  3  \w    -76.00  21.00   1.00   70.34    --  -10.40 -77.00  60.00   97
  4  \w    -12.00  14.00   1.00   70.34    --   11.41 -99.00 120.00   26
;
_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      0.0488617000
_diffrn_orient_matrix_UB_12      0.0284161000
_diffrn_orient_matrix_UB_13      0.0081240000
_diffrn_orient_matrix_UB_21      -0.0342720000
_diffrn_orient_matrix_UB_22      0.0425127000
_diffrn_orient_matrix_UB_23      -0.0017237000
_diffrn_orient_matrix_UB_31      -0.0141427000
_diffrn_orient_matrix_UB_32      -0.0048865000
_diffrn_orient_matrix_UB_33      0.0321776000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27858
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.567
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83536
_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    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8500
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0282P)^2^+2.2574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4030
_reflns_number_total             4515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py00395e2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1549377--1549380.cif.'
_cod_database_code               1549379
_chemical_oxdiff_formula         'C H N O Pd Cl'
_chemical_oxdiff_usercomment     anp-dipp-PdCl2
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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) groups
2.a Riding coordinates:
 O1(H1B)
2.b Ternary CH refined with riding coordinates:
 N1(H1), C1(H1A), C14(H14), C17(H17)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C11(H11), C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              4089
_shelx_shelxl_version_number     2014/7
_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 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.721