Ligand and solvent control of selectivity in the C-H activation of a pyridylimine-substituted 1-naphthalene; a combined synthetic and computational study.
Simayi, Rena; Gillbard, Simone M.; Cross, Warren B.; Hope, Eric G.; Singh, Kuldip; Solan, Gregory A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11680–11690; doi:10.1039/c8dt02565g

data_7047220
_publ_section_title
;
 Ligand and solvent control of selectivity in the C-H activation of a
 pyridylimine-substituted 1-naphthalene; a combined synthetic and
 computational study.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11680
_journal_page_last               11690
_journal_paper_doi               10.1039/c8dt02565g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C29 H30 Cl2 N2 Pd, 2(C H Cl3)'
_chemical_formula_sum            'C31 H32 Cl8 N2 Pd'
_chemical_formula_weight         822.58
_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_method           SHELXL-2018/3
_audit_update_record
;
2018-08-01 deposited with the CCDC.
2018-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                88.721(3)
_cell_angle_beta                 77.111(3)
_cell_angle_gamma                76.355(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8725(12)
_cell_length_b                   12.8984(18)
_cell_length_c                   15.781(2)
_cell_measurement_reflns_used    764
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.306
_cell_measurement_theta_min      2.488
_cell_volume                     1709.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_av_unetI/netI     0.2669
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13501
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         1.324
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absoprtion correction based on 2269 reflections(SADABS);Rint 0.1013 before
correction and 0.0578 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0336P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3065
_reflns_number_total             6628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02565g3.cif
_cod_data_source_block           16046
_cod_depositor_comments
'Adding full bibliography for 7047219--7047222.cif.'
_cod_database_code               7047220
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;

The crystal data was v weak due to crystal quality.

;
_shelx_res_checksum              29713