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_7042750
_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_sum            'C40 H26 Cl2 N3 O6 P3'
_chemical_formula_weight         808.45
_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
;
2016-09-24 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.834(4)
_cell_angle_beta                 96.273(4)
_cell_angle_gamma                106.767(5)
_cell_formula_units_Z            2
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_cell_length_b                   13.1019(6)
_cell_length_c                   16.2731(7)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      3.1
_cell_volume                     1795.52(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16019
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.959
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Numabs Rigaku 1999'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0576
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_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^)+(0.0640P)^2^+1.6230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5463
_reflns_number_total             6317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00737j2.cif
_cod_data_source_block           msb-vsk-233_mo
_cod_original_cell_volume        1795.51(16)
_cod_database_code               7042750
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              46105