New insight into solid-state molecular dynamics: mechanochemical synthesis of azobenzene/triphenylphosphine palladacycles
Dominik Cincic; Marina Juribasic; Darko Babic; Kresimir Molcanov; Primoz Sket; Janez Plavec; Manda Curic; Chem.Commun. 47 (2011) 11543–; doi:10.1039/c1cc15377c

data_7106963
_publ_section_title
;
 New insight into solid-state molecular dynamics: mechanochemical
 synthesis of azobenzene/triphenylphosphine palladacycles
;
_journal_name_full               Chem.Commun.
_journal_page_first              11543
_journal_paper_doi               10.1039/c1cc15377c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C48 H38 Cl2 N2 P2 Pd2, C2 H6 O'
_chemical_formula_sum            'C50 H44 Cl2 N2 O P2 Pd2'
_chemical_formula_weight         1034.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2010-10-14T17:35:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.9830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.62710(10)
_cell_length_b                   9.02440(10)
_cell_length_c                   43.0468(4)
_cell_measurement_reflns_used    16686
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.0964
_cell_measurement_theta_min      3.0933
_cell_volume                     4492.19(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Oxford Xcalibur Nova'
_diffrn_measurement_method
;
CCD detector
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            22989
_diffrn_reflns_theta_full        76.21
_diffrn_reflns_theta_max         76.21
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    8.532
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.40374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.53
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.996
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         9219
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_gt           0.064
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+51.5395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                8513
_reflns_number_total             9219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15377c.txt
_cod_data_source_block           manda-c2abtpp
_cod_database_code               7106963