First examples of tri- and tetraphosphametacyclophanes: synthesis and isolation of an unusual hexapalladium complex containing pincer units with Pd—P covalent bonds
Kashid, Vitthal S.; Radhakrishna, Latchupatula; Balakrishna, Maravanji Shivaramaiah; Dalton Trans.  (2017) –; doi:10.1039/C7DT00737J

data_7042748
_publ_section_title
;
 First examples of tri- and tetraphosphametacyclophanes: synthesis and
 isolation of an unusual hexapalladium complex containing pincer units
 with Pd---P covalent bonds
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00737J
_journal_year                    2017
_chemical_formula_moiety         'C44 H36 Cl6 N2 O4 P4 Pd6'
_chemical_formula_sum            'C44 H36 Cl6 N2 O4 P4 Pd6'
_chemical_formula_weight         1631.73
_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-2014/7
_audit_update_record
;
2017-02-11 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                102.789(2)
_cell_angle_beta                 95.8839(19)
_cell_angle_gamma                113.851(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0974(2)
_cell_length_b                   10.1677(3)
_cell_length_c                   13.9117(3)
_cell_measurement_reflns_used    18735
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.1890
_cell_measurement_theta_min      2.2500
_cell_volume                     1244.02(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku saturn 724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0271
_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       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22657
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.288
_exptl_absorpt_coefficient_mu    2.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48285
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS RIGAKU 1999'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4353
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0318P)^2^+2.2641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4043
_reflns_number_total             4353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00737j2.cif
_cod_data_source_block           MSB-VSK-294
_cod_original_cell_volume        1244.01(6)
_cod_database_code               7042748
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              43538