Polymer [Pd(CH2SO2C6H4Me)2]n, a precursor to remarkably stable Pd organometallics
Pérez-Briso, Celeste; Gallego, Ana M.; Martín-Alvarez, Jose M.; Martínez-Ilarduya, Jesús M.; Espinet, Pablo; Dalton Trans.  (2017) –; doi:10.1039/C7DT00904F

data_7043306
_publ_section_title
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 Polymer [Pd(CH2SO2C6H4Me)2]n, a precursor to remarkably stable Pd
 organometallics
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00904F
_journal_year                    2017
_chemical_formula_moiety         'C34 H36 N O4 P Pd S2'
_chemical_formula_sum            'C34 H36 N O4 P Pd S2'
_chemical_formula_weight         724.13
_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             2017-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
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2017-02-19 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                91.407(5)
_cell_angle_beta                 99.846(4)
_cell_angle_gamma                103.932(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5024(5)
_cell_length_b                   12.4119(9)
_cell_length_c                   13.1782(8)
_cell_measurement_reflns_used    5536
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.8410
_cell_measurement_theta_min      2.6400
_cell_volume                     1638.86(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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_temperature      296.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.820
_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     -9.00  85.00   1.00   19.36    --   11.82  57.00 -60.00   94
  2  \w    -15.00  74.00   1.00   19.36    --   11.82  77.00  60.00   89
  3  \w      2.00  28.00   1.00   19.36    --   11.82 -99.00 150.00   26
  4  \w    -54.00  40.00   1.00   19.36    --   11.82 -57.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0008850000
_diffrn_orient_matrix_UB_12      -0.0034995000
_diffrn_orient_matrix_UB_13      0.0537474000
_diffrn_orient_matrix_UB_21      -0.0149134000
_diffrn_orient_matrix_UB_22      0.0526611000
_diffrn_orient_matrix_UB_23      0.0027169000
_diffrn_orient_matrix_UB_31      -0.0691751000
_diffrn_orient_matrix_UB_32      -0.0264144000
_diffrn_orient_matrix_UB_33      -0.0101125000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.889
_diffrn_reflns_theta_min         2.032
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0316P)^2^+0.2115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5628
_reflns_number_total             7775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00904f2.cif
_cod_data_source_block           11
_cod_original_cell_volume        1638.87(18)
_cod_database_code               7043306
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C34 H36 N O4 P S2 Pd'
_chemical_oxdiff_usercomment     colourless
_cell_oxdiff_angle_alpha         91.407(5)
_cell_oxdiff_angle_beta          99.846(4)
_cell_oxdiff_angle_gamma         103.932(5)
_cell_oxdiff_length_a            10.5024(5)
_cell_oxdiff_length_b            12.4119(9)
_cell_oxdiff_length_c            13.1782(8)
_cell_oxdiff_measurement_reflns_used 5536
_cell_oxdiff_volume              1638.87(17)
_reflns_odcompleteness_completeness 99.96
_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 C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              89120
_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 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.617