Synthesis of mesoporous metal complex-silica materials and their use as solvent-free catalysts
Linares, Noemi; Sepúlveda, Angel E.; Pacheco, María C.; Berenguer, Jesús R.; Lalinde, Elena; Nájera, Carmen; Garcia-Martinez, Javier; New Journal of Chemistry 35 (2011) 225–; doi:10.1039/c0nj00509f

data_7052541
_publ_section_title
;
 Synthesis of mesoporous metal complex-silica materials and their use
 as solvent-free catalysts
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              225
_journal_paper_doi               10.1039/c0nj00509f
_journal_volume                  35
_journal_year                    2011
_chemical_formula_sum            'C40 H58 Cl2 O6 P2 Pd Si2'
_chemical_formula_weight         930.28
_chemical_name_common            'Compound X'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-01-18T19:43:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                76.248(3)
_cell_angle_beta                 71.031(4)
_cell_angle_gamma                78.739(3)
_cell_formula_units_Z            1
_cell_length_a                   9.2480(4)
_cell_length_b                   11.4080(7)
_cell_length_c                   11.7210(8)
_cell_measurement_reflns_used    1705
_cell_measurement_temperature    120.0(10)
_cell_volume                     1126.49(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0260621
_diffrn_orient_matrix_UB_12      0.0904972
_diffrn_orient_matrix_UB_13      -0.0172153
_diffrn_orient_matrix_UB_21      0.1022515
_diffrn_orient_matrix_UB_22      0.0095226
_diffrn_orient_matrix_UB_23      0.0062285
_diffrn_orient_matrix_UB_31      0.0464758
_diffrn_orient_matrix_UB_32      0.0007955
_diffrn_orient_matrix_UB_33      -0.0900054
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.061
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13908
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4607
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.9618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.078
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                3775
_reflns_number_total             4607
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0NJ00509F.TXT
_cod_data_source_block           aes256
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        1126.49(11)
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               7052541