Structural and conformational changes in [M(1,10-diaza-18-crown-6)Cl2] (M = Pd, Pb) complexes: a crystallographic and theoretical study
Arenaza-Corona, Antonino; Morales-Morales, David; Hernández-Ahuactzi, Iran F.; Barba, Victor; CrystEngComm 20 (2018) 6733–; doi:10.1039/C8CE01478G

data_7231569
_publ_section_title
;
 Structural and conformational changes in [M(1,10-diaza-18-crown-6)Cl2] (M
 = Pd, Pb) complexes: a crystallographic and theoretical study
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6733
_journal_paper_doi               10.1039/C8CE01478G
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C12 H26 Cl2 N2 O4 Pd'
_chemical_formula_sum            'C12 H26 Cl2 N2 O4 Pd'
_chemical_formula_weight         439.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-07-10 deposited with the CCDC.
2018-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                83.909(3)
_cell_angle_beta                 81.020(3)
_cell_angle_gamma                87.767(3)
_cell_formula_units_Z            1
_cell_length_a                   6.5577(3)
_cell_length_b                   7.8482(3)
_cell_length_c                   7.8785(3)
_cell_measurement_reflns_used    5580
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9800
_cell_measurement_theta_min      3.1330
_cell_volume                     398.14(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
  1 omega   -1.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000    0.0000 84

  2 omega  -52.00   42.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -77.0000 -120.0000 94

  3 omega   -4.00   84.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   38.0000 -180.0000 88

  4 omega   -1.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000   30.0000 84

  5 omega  -83.00    1.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  -57.0000   30.0000 84

  6 omega  -27.00   20.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  -93.0000  135.0000 47

  7 omega  -20.00   54.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -99.0000    0.0000 74

  8 omega   34.00   88.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374 -178.0000 -120.0000 54

  9 omega   -1.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000  -90.0000 84

 10 omega  -20.00   54.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -99.0000  150.0000 74

 11 omega  -54.00   34.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -38.0000   30.0000 88

 12 omega  -54.00   34.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -38.0000    0.0000 88

 13 omega  -52.00  -12.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.0187   93.0000 -112.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0419045000
_diffrn_orient_matrix_UB_12      0.0820995000
_diffrn_orient_matrix_UB_13      0.0175739000
_diffrn_orient_matrix_UB_21      0.0891408000
_diffrn_orient_matrix_UB_22      0.0172042000
_diffrn_orient_matrix_UB_23      0.0354556000
_diffrn_orient_matrix_UB_31      0.0479106000
_diffrn_orient_matrix_UB_32      0.0350578000
_diffrn_orient_matrix_UB_33      -0.0826315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8570
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.147
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       prism
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.2810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1859
_reflns_number_total             1929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01478g1.cif
_cod_data_source_block           e55vb
_cod_depositor_comments
'Adding full bibliography for 7231567--7231569.cif.'
_cod_original_cell_volume        398.15(3)
_cod_database_code               7231569
_chemical_oxdiff_formula         'C H O N S Rb'
_reflns_odcompleteness_completeness 100.00
_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, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C1(H1A,H1B), C3(H3B,H3A), C2(H2A,H2B), C5(H5A,H5B)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-09
_olex2_submission_special_instructions 'No special instructions were received'