Epitaxial Retrieval of a Disappearing Polymorph.
Tidey, Jeremiah P.; O'Connor, Alice E; Markevich, Alexander; Bichoutskaia, Elena; Cavan, Joseph J. P.; Lawrance, Geoffrey A.; Wong, Henry L. S.; McMaster, Jonathan; Schröder, Martin; Blake, Alexander J.; Crystal growth & design 15 (2015) 115–123; doi:10.1021/cg500967w

data_4512494
_publ_section_title
;
 Epitaxial Retrieval of a Disappearing Polymorph.
;
_journal_issue                   1
_journal_name_full               'Crystal growth &amp; design'
_journal_page_first              115
_journal_page_last               123
_journal_paper_doi               10.1021/cg500967w
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C6 H12 Cl2 O Pd S2'
_chemical_formula_sum            'C6 H12 Cl2 O Pd S2'
_chemical_formula_weight         341.58
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.785(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.02123(16)
_cell_length_b                   11.4020(3)
_cell_length_c                   13.3817(3)
_cell_measurement_reflns_used    2505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1790
_cell_measurement_theta_min      3.4070
_cell_volume                     1063.78(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
  1 omega  -54.00  -27.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.8594  -57.0000  120.0000 27

  2 omega  -30.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6740   37.0000   90.0000 123

  3 omega   60.00  114.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6740  179.0000   60.0000 54

  4 omega   -3.00  103.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6740   57.0000  -60.0000 106

  5 omega   -4.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6740   57.0000  150.0000 98

  6 omega  -14.00   27.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3928  -99.0000    0.0000 41

  7 omega  -18.00   11.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3928  -99.0000  -60.0000 29

  8 omega    1.00   42.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3928   77.0000  -90.0000 41
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0147897000
_diffrn_orient_matrix_UB_12      -0.0582628000
_diffrn_orient_matrix_UB_13      0.0159788000
_diffrn_orient_matrix_UB_21      -0.0456743000
_diffrn_orient_matrix_UB_22      0.0217603000
_diffrn_orient_matrix_UB_23      0.0407564000
_diffrn_orient_matrix_UB_31      -0.0897118000
_diffrn_orient_matrix_UB_32      -0.0014477000
_diffrn_orient_matrix_UB_33      -0.0305242000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7692
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.079
_diffrn_reflns_theta_min         3.135
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.590
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration
over a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.1106
_exptl_crystal_size_mid          0.0995
_exptl_crystal_size_min          0.0195
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2390
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0283P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1782
_reflns_number_total             2390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg500967w_si_002.cif
_cod_data_source_block           cPd
_cod_depositor_comments
'Adding full bibliography for 4512492--4512497.cif.'
_cod_original_cell_volume        1063.78(5)
_cod_database_code               4512494
_shelxl_version_number           2012-9
_chemical_oxdiff_formula         'Pd1 S2 O1 Cl2 C6 H12'
_chemical_oxdiff_usercomment     'MeNO2 / Et2O warm'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C3-C2 = C6-C5
 1.52 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C8(H8A,H8B)
;
_shelx_res_checksum              23112
_shelx_hkl_checksum              31676
_olex2_submission_special_instructions 'No special instructions were received'