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_7019541
_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         'C54 H52 Cu2 N4 P2 S2'
_chemical_formula_sum            'C54 H52 Cu2 N4 P2 S2'
_chemical_formula_weight         1010.14
_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             2010-04-20T12:06:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.168(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.107(5)
_cell_length_b                   9.505(5)
_cell_length_c                   16.249(5)
_cell_measurement_reflns_used    35667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.5554
_cell_measurement_theta_min      3.769
_cell_volume                     2412.0(17)
_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    '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 0.996
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Oxford Diffraction Gemini, Ruby ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0030174627
_diffrn_orient_matrix_UB_12      -0.0418882165
_diffrn_orient_matrix_UB_13      -0.0367428363
_diffrn_orient_matrix_UB_21      0.0439012656
_diffrn_orient_matrix_UB_22      -0.0180664504
_diffrn_orient_matrix_UB_23      0.0144157559
_diffrn_orient_matrix_UB_31      -0.0112894348
_diffrn_orient_matrix_UB_32      -0.0590558538
_diffrn_orient_matrix_UB_33      0.0216547502
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            93483
_diffrn_reflns_theta_full        37
_diffrn_reflns_theta_max         37.67
_diffrn_reflns_theta_min         3.83
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.625
_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    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         12473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                9359
_reflns_number_total             12473
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt30579h.txt
_cod_data_source_block           rip3_clless
_cod_original_cell_volume        2412.0(16)
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_database_code               7019541