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_7231568
_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 Pb'
_chemical_formula_sum            'C12 H26 Cl2 N2 O4 Pb'
_chemical_formula_weight         540.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-07-10 deposited with the CCDC.
2018-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.063(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.46450(19)
_cell_length_b                   7.6682(2)
_cell_length_c                   16.3035(5)
_cell_measurement_reflns_used    2092
_cell_measurement_temperature    100.29(10)
_cell_measurement_theta_max      28.6920
_cell_measurement_theta_min      3.8750
_cell_volume                     918.84(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.29(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_details
;
  1 omega    3.00   87.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -       15.2374   19.0000  -90.0000 84

  2 omega  -17.00   30.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -99.0000  -30.0000 47

  3 omega  -64.00  -20.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  -38.0000   60.0000 44

  4 omega  -71.00  -31.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  138.0000 -150.0000 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      -0.0177970000
_diffrn_orient_matrix_UB_12      -0.0036653000
_diffrn_orient_matrix_UB_13      -0.0441394000
_diffrn_orient_matrix_UB_21      0.0399858000
_diffrn_orient_matrix_UB_22      -0.0841133000
_diffrn_orient_matrix_UB_23      0.0013880000
_diffrn_orient_matrix_UB_31      -0.0860260000
_diffrn_orient_matrix_UB_32      -0.0383363000
_diffrn_orient_matrix_UB_33      0.0011142000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4040
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         2.771
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50967
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0119P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1623
_reflns_number_total             2134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01478g1.cif
_cod_data_source_block           e97vb
_cod_depositor_comments
'Adding full bibliography for 7231567--7231569.cif.'
_cod_database_code               7231568
_chemical_oxdiff_formula         'C H O S N Pd P Cl'
_reflns_odcompleteness_completeness 99.90
_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), C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-26
_olex2_submission_special_instructions 'No special instructions were received'