A trans-bidentate bis-pyridinyl ligand with a transition metal hinge
Vieira, Noah Christopher; Pienkos, Jared A.; McMillen, Colin; Myers, Alexis R.; Clay, Alyssa Paige; Wagenknecht, Paul S.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03252H

data_7044502
_publ_section_title
;
 A trans-bidentate bis-pyridinyl ligand with a transition metal hinge
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03252H
_journal_year                    2017
_chemical_formula_sum            'C35 H39.5 Cl2 N2.5 Pd Ti'
_chemical_formula_weight         720.39
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-28 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                104.000(2)
_cell_angle_beta                 93.8680(10)
_cell_angle_gamma                96.8550(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8432(3)
_cell_length_b                   12.3352(5)
_cell_length_c                   16.4088(7)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.39
_cell_volume                     1715.69(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27680
_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         26.065
_diffrn_reflns_theta_min         2.331
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       column
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6778
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0609P)^2^+2.0045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5513
_reflns_number_total             6778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03252h2.cif
_cod_data_source_block           d8-1831_a
_cod_original_formula_sum        'C35 H39.50 Cl2 N2.50 Pd Ti'
_cod_database_code               7044502
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              9559