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_7106964
_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         '2(C50 H42 Cl2 N4 O2 P2 Pd2), C2 H6 O, H2 O'
_chemical_formula_sum            'C51 H46 Cl2 N4 O3 P2 Pd2'
_chemical_formula_weight         1108.56
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2010-10-28T16:43:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                110.178(3)
_cell_angle_beta                 90.883(2)
_cell_angle_gamma                90.024(3)
_cell_formula_units_Z            4
_cell_length_a                   10.0943(3)
_cell_length_b                   20.0688(7)
_cell_length_c                   25.3224(6)
_cell_measurement_reflns_used    13321
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.9554
_cell_measurement_theta_min      3.4576
_cell_volume                     4814.3(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54179
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43140
_diffrn_reflns_theta_full        76.14
_diffrn_reflns_theta_max         76.14
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    8.048
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.33114
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.91
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         19491
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+60.5558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2358
_reflns_number_gt                9835
_reflns_number_total             19491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15377c.txt
_cod_data_source_block           manda-4a-d12-ponovo
_cod_original_cell_volume        4814.3(2)
_cod_database_code               7106964