Rational Design of Porous Coordination Polymers Based on Bis(phosphine)MCl2 Complexes That Exhibit High-Temperature H2 Sorption and Chemical Reactivity
Alisha M. Bohnsack; Ilich A. Ibarra; Vladimir I. Bakhmutov; Vincent M. Lynch; Simon M. Humphrey; Journal of the American Chemical Society 135 (2013) 16038–16041; doi:10.1021/ja408508m

data_4121063
_publ_contact_author             'Dr. Simon M. Humphrey'
_publ_contact_author_email       smh@cm.utexas.edu
_publ_section_title
;
 Rational Design of Porous Coordination Polymers Based on
 Bis(phosphine)MCl2 Complexes That Exhibit High-Temperature H2 Sorption
 and Chemical Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16038
_journal_page_last               16041
_journal_paper_doi               10.1021/ja408508m
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C34 H24 Cl2 O10 P2 Pd Zn2'
_chemical_formula_sum            'C34 H24 Cl2 O10 P2 Pd Zn2'
_chemical_formula_weight         962.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           74
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9532(19)
_cell_length_b                   25.725(2)
_cell_length_c                   14.8141(12)
_cell_measurement_reflns_used    11614
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      1.6
_cell_volume                     9128.4(13)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support loop
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58427
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.60
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.700
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4203
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1738
_refine_ls_R_factor_gt           0.1082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1886P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2722
_refine_ls_wR_factor_ref         0.3180
_reflns_number_gt                2646
_reflns_number_total             4203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408508m_si_003.cif
_cod_data_source_block           sh12012fs
_cod_original_cell_volume        9128.2(13)
_cod_database_code               4121063