Mechanochemical and solution synthesis, X-ray structure and IR and (31)P solid state NMR spectroscopic studies of copper(i) thiocyanate adducts with bulky monodentate tertiary phosphine ligands.
Bowmaker, Graham A.; Hanna, John V.; Hart, Robert D.; Healy, Peter C.; King, Scott P.; Marchetti, Fabio; Pettinari, Claudio; Skelton, Brian W.; Tabacaru, Aurel; White, Allan H.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 7513–7525; doi:10.1039/c2dt30579h

data_7019543
_publ_section_title
;
 Mechanochemical and solution synthesis, X-ray structure and IR and (31)P
 solid state NMR spectroscopic studies of copper(i) thiocyanate adducts
 with bulky monodentate tertiary phosphine ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7513
_journal_page_last               7525
_journal_paper_doi               10.1039/c2dt30579h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C48 H48 Cu2 N4 P2 S2'
_chemical_formula_sum            'C48 H48 Cu2 N4 P2 S2'
_chemical_formula_weight         934.04
_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             2010-07-16T15:11:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.068(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3118(2)
_cell_length_b                   17.5977(4)
_cell_length_c                   13.3941(4)
_cell_measurement_reflns_used    10520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.4242
_cell_measurement_theta_min      3.6319
_cell_volume                     2154.02(10)
_computing_cell_refinement
;

CrysAlisPro, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov 6 2009,16:24:50)

;
_computing_data_collection
;

CrysAlisPro, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov 6 2009,16:24:50)

;
_computing_data_reduction
;

CrysAlisPro, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov 6 2009,16:24:50)

;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0246332323
_diffrn_orient_matrix_UB_12      0.0133105175
_diffrn_orient_matrix_UB_13      0.04359274
_diffrn_orient_matrix_UB_21      0.011605905
_diffrn_orient_matrix_UB_22      0.0378701899
_diffrn_orient_matrix_UB_23      -0.0142688652
_diffrn_orient_matrix_UB_31      -0.0724263097
_diffrn_orient_matrix_UB_32      0.0015052826
_diffrn_orient_matrix_UB_33      -0.0280771132
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27484
_diffrn_reflns_theta_full        32.25
_diffrn_reflns_theta_max         33.52
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;

CrysAlisPro, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov 6 2009,16:24:50)

Analytical numeric absorption correction using a multifaceted crystal

model based on expressions derived by R.C. Clark & J.S.

(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.44
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         7971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                5502
_reflns_number_total             7971
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt30579h.txt
_cod_data_source_block           cpots
_cod_original_cell_volume        2154.02(9)
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_database_code               7019543