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_7043303
_publ_section_title
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 Polymer [Pd(CH2SO2C6H4Me)2]n, a precursor to remarkably stable Pd
 organometallics
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00904F
_journal_year                    2017
_chemical_formula_moiety         'C68 H70 N2 O8 P2 Pd2 S4, 3(C H2 Cl2)'
_chemical_formula_sum            'C71 H76 Cl6 N2 O8 P2 Pd2 S4'
_chemical_formula_weight         1701.01
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-19 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1345(2)
_cell_length_b                   18.0323(2)
_cell_length_c                   14.4143(2)
_cell_measurement_reflns_used    9246
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      29.6480
_cell_measurement_theta_min      2.2650
_cell_volume                     3661.19(8)
_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_environment      N~2~
_diffrn_ambient_temperature      150.05(10)
_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 0.839
_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    -12.00  29.00   1.00   19.16    --  -10.11 -99.00 -60.00   41
  2  \w     33.00  82.00   1.00   19.16    --   11.82  37.00-120.00   49
  3  \w    -20.00  89.00   1.00   19.16    --   11.82  19.00-180.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0155241000
_diffrn_orient_matrix_UB_12      -0.0356972000
_diffrn_orient_matrix_UB_13      -0.0127993000
_diffrn_orient_matrix_UB_21      0.0399918000
_diffrn_orient_matrix_UB_22      0.0031652000
_diffrn_orient_matrix_UB_23      0.0328793000
_diffrn_orient_matrix_UB_31      -0.0263569000
_diffrn_orient_matrix_UB_32      -0.0162365000
_diffrn_orient_matrix_UB_33      0.0345382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20462
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.856
_diffrn_reflns_theta_min         2.107
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   gaussian
_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    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8839
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0228P)^2^+3.6659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7191
_reflns_number_total             8839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00904f2.cif
_cod_data_source_block           14
_cod_database_code               7043303
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C35 H38 Cl3 P S2 O4 Pd N'
_chemical_oxdiff_usercomment     colourless
_reflns_odcompleteness_completeness 99.91
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Cl4, C92, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim C92 \\sim Cl3: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Fixed Sof: Cl4(0.5) C92(0.5) H92A(0.5) H92B(0.5) Cl3(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C91(H91A,H91B), C92(H92A,H92B)
5.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)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              15330
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.873