The role of short-range diffusion in solvent-assisted mechanochemical synthesis of metal complexes
Bowmaker, Graham A.; Hanna, John V.; Hart, Robert D.; Skelton, Brian W.; White, Allan H.; Dalton Transactions  (2008) 5290–5292; doi:10.1039/b810659m

data_7004698
_publ_section_title
;
 The role of short-range diffusion in solvent-assisted mechanochemical
 synthesis of metal complexes
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              5290
_journal_page_last               5292
_journal_paper_doi               10.1039/b810659m
_journal_year                    2008
_chemical_formula_moiety         'C74 H60 Cu2 N2 P4 S2'
_chemical_formula_sum            'C74 H60 Cu2 N2 P4 S2'
_chemical_formula_weight         1292.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-03-07T13:02:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.453(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6170(4)
_cell_length_b                   13.5021(2)
_cell_length_c                   20.1922(3)
_cell_measurement_reflns_used    26063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.0965
_cell_measurement_theta_min      2.3314
_cell_volume                     6206.10(18)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      -0.0326423332
_diffrn_orient_matrix_UB_12      0.0230037365
_diffrn_orient_matrix_UB_13      -0.0060677133
_diffrn_orient_matrix_UB_21      -0.0039669444
_diffrn_orient_matrix_UB_22      -0.0167507817
_diffrn_orient_matrix_UB_23      0.0272129534
_diffrn_orient_matrix_UB_31      0.0155324866
_diffrn_orient_matrix_UB_32      0.0439952854
_diffrn_orient_matrix_UB_33      0.0135711597
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            119784
_diffrn_reflns_theta_full        34.25
_diffrn_reflns_theta_max         35.19
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.93996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.79
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         26401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                14188
_reflns_number_total             26401
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b810659m.txt
_cod_data_source_block           gb0809
_cod_original_cell_volume        6206.10(17)
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_database_code               7004698