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_7047222
_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         'C28 H28 Cl2 N2 Pd,C H2 Cl2'
_chemical_formula_sum            'C29 H30 Cl4 N2 Pd'
_chemical_formula_weight         654.75
_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
_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                90
_cell_angle_beta                 90.37(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.060(2)
_cell_length_b                   11.775(2)
_cell_length_c                   23.032(5)
_cell_measurement_reflns_used    366
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.428
_cell_measurement_theta_min      2.468
_cell_volume                     2728.2(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.3807
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5363
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.204
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 1509 reflections(SADABS);Rint 0.1281 before
correction and 0.0677 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;

Disordered CH2Cl2 was omitted using the SQUEEZE option of PLATON.The
solvent accessible voids are 375.5 \%A3 with an estimated 163e/cell
to be added. Four solvent CH2Cl2 molecules/unit cell accounting for
168e were included in the formula, FWt, (000) and density calculations. 
PLATON Reference: Spek, A.L. (1990), Acta Cryst.

;
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.715
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.715
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0159P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1775
_reflns_number_total             5363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02565g3.cif
_cod_data_source_block           16043
_cod_depositor_comments
'Adding full bibliography for 7047219--7047222.cif.'
_cod_database_code               7047222
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
The crystal data was weak due to crystal quality.
;
_shelx_res_checksum              79929