Cyclometallated Platinum(II) and Palladium(II) Complexes Containing 1,5-Diarylbiguanides: Synthesis, Characterisation and Hydrogen Bond-directed Assembly
McMorran, David; McKay, Aidan P.; Gordon, Keith; Shillito, Georgina E.; CrystEngComm  (2017) –; doi:10.1039/C7CE01805C

data_7229569
_publ_section_title
;
 Cyclometallated Platinum(II) and Palladium(II) Complexes Containing
 1,5-Diarylbiguanides: Synthesis, Characterisation and Hydrogen
 Bond-directed Assembly
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01805C
_journal_year                    2017
_chemical_formula_sum            'C35 H42 N6 O2 Pd'
_chemical_formula_weight         685.14
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                79.325(2)
_cell_angle_beta                 77.329(3)
_cell_angle_gamma                73.188(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6109(3)
_cell_length_b                   12.3786(3)
_cell_length_c                   13.1939(4)
_cell_measurement_reflns_used    19913
_cell_measurement_temperature    100.00(1)
_cell_measurement_theta_max      73.5420
_cell_measurement_theta_min      3.6800
_cell_volume                     1604.70(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(1)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22434
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        68.500
_diffrn_reflns_theta_max         73.515
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.988
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.2640
_exptl_crystal_size_mid          0.1238
_exptl_crystal_size_min          0.0488
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6361
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.9008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6228
_reflns_number_total             6361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01805c2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7229569
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              30470