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_7042749
_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         'C56 H42 N4 O9 P4'
_chemical_formula_sum            'C56 H42 N4 O9 P4'
_chemical_formula_weight         1038.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 97.725(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9200(3)
_cell_length_b                   19.0391(8)
_cell_length_c                   20.9881(6)
_cell_measurement_reflns_used    9587
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.6190
_cell_measurement_theta_min      3.1250
_cell_volume                     5115.9(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rigaku saturn 724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.1054
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28013
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.767
_diffrn_reflns_theta_min         3.147
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61938
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Numabs Rigaku 1999'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         9815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0819
_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^)+(0.1449P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6159
_reflns_number_total             9815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00737j2.cif
_cod_data_source_block           MSB-VSK-292
_cod_database_code               7042749
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              20955