Highly soluble Cu(i)-acetonitrile salts as building blocks for novel phosphorus-rich organometallic-inorganic compounds.
Elsayed Moussa, Mehdi; Piesch, Martin; Fleischmann, Martin; Schreiner, Andrea; Seidl, Michael; Scheer, Manfred; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16031–16035; doi:10.1039/c8dt03723j

data_7047765
_publ_section_title
;
 Highly soluble Cu(i)-acetonitrile salts as building blocks for novel
 phosphorus-rich organometallic-inorganic compounds.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16031
_journal_page_last               16035
_journal_paper_doi               10.1039/c8dt03723j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'2(Al1 C36 F46 O3), 2(C3 H4.5 Cu0.5 N1.5), C8 H12 Cu1 N4, 2.98(C H2 Cl2)'
_chemical_formula_sum            'C88.98 H26.96 Al2 Cl5.96 Cu2 F92 N7 O6'
_chemical_formula_weight         3430.22
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-07 deposited with the CCDC.
2018-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   14.36351(9)
_cell_length_b                   14.36351(9)
_cell_length_c                   15.72381(12)
_cell_measurement_reflns_used    32363
_cell_measurement_temperature    123.1(3)
_cell_measurement_theta_max      65.7680
_cell_measurement_theta_min      4.5120
_cell_volume                     2809.37(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -54.00  -28.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0288  125.0000 -120.0000 52

  2 omega   11.00   99.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0288   38.0000  -60.0000 176

  3 omega  -35.00   68.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega    1.00   87.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0288 -125.0000   90.0000 172

  5 omega -157.00 -131.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  178.0000 -180.0000 52

  6 omega -155.00 -129.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  178.0000    0.0000 52

  7 omega   57.00  102.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000  -12.5474 90

  8 omega   81.00  107.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   88.1135 52

  9 omega   28.00   54.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -173.8797 52

 10 omega  112.00  138.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  150.0000 52

 11 omega  141.00  167.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  150.0000 52

 12 omega   64.00   90.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 52

 13 omega   96.00  170.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 148

 14 omega   91.00  168.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000   90.0000 154

 15 omega   69.00  128.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -89.0000   37.2906 118

 16 omega   51.00   77.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   88.1135 52

 17 omega   52.00   84.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000 -120.0000 64

 18 omega   23.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000 -120.0000 52

 19 omega   53.00   79.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000  -30.0000 52

 20 omega   30.00   77.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 94

 21 omega   48.00   76.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  120.0000 56

 22 omega   30.00   81.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  -30.0000 102

 23 omega   15.00   41.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000   90.0000 52

 24 omega   55.00   81.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000   90.0000 52

 25 omega   20.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   30.0000 88

 26 omega   30.00   56.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -60.0000 52

 27 omega   14.00   39.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  150.0000 50

 28 omega   58.00   84.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000  -90.0000 52

 29 omega   24.00   61.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -89.0000   37.2906 74

 30 omega   84.00  109.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   90.0000 50

 31 omega   18.00   43.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000    0.0000 50

 32 omega   37.00   63.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   90.0000 52

 33 omega   14.00   60.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   90.0000 92

 34 omega   50.00   76.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   60.0000 52

 35 omega   39.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 50

 36 omega  130.00  170.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -180.0000 80

 37 omega   64.00   91.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 54

 38 omega  127.00  170.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 86

 39 omega   24.00   68.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -90.0000 88

 40 omega   98.00  126.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -88.0000   84.7152 56

 41 omega   36.00   62.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   18.0000   11.5064 52

 42 omega  147.00  173.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   18.0000   11.5064 52

 43 omega   86.00  129.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -173.8797 86

 44 omega  122.00  168.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000 -180.0000 92

 45 omega   26.00   69.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -30.0000 86

 46 omega   25.00   76.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 102

 47 omega   26.00   52.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -120.0000 52

 48 omega   94.00  134.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000  -89.9199 80

 49 omega   79.00  105.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000  -60.0000 52

 50 omega  147.00  173.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -120.0000 52

 51 omega   55.00   81.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000 -180.0000 52

 52 omega   17.00   42.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000   30.0000 50

 53 omega   24.00   69.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000  -89.9199 90

 54 omega -122.00   -5.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0288  -77.0000   30.0000 234

 55 omega -122.00   -5.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0288  -77.0000  -90.0000 234

 56 omega    5.00  122.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0288   77.0000 -180.0000 234

 57 omega   -3.00   96.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0288 -125.0000  -30.0000 198

 58 omega    9.00  116.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0288   57.0000  120.0000 214

 59 omega    9.00  116.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0288   57.0000   30.0000 214

 60 omega -169.00  -74.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -71.0000   10.5751 190

 61 omega -166.00  -58.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -61.0000  120.0000 216

 62 omega   16.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
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 63 omega   59.00  175.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
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 64 omega   59.00  175.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 232
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0382310000
_diffrn_orient_matrix_UB_12      0.0238410000
_diffrn_orient_matrix_UB_13      0.0845674000
_diffrn_orient_matrix_UB_21      -0.0924286000
_diffrn_orient_matrix_UB_22      -0.1174295000
_diffrn_orient_matrix_UB_23      0.0040068000
_diffrn_orient_matrix_UB_31      0.0730257000
_diffrn_orient_matrix_UB_32      -0.0312009000
_diffrn_orient_matrix_UB_33      0.0493316000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54098
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        65.981
_diffrn_reflns_theta_max         65.981
_diffrn_reflns_theta_min         3.553
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.895
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_F_000             1671
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.2061
_exptl_crystal_size_min          0.1829
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         3271
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.9408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3049
_reflns_number_total             3271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03723j2.cif
_cod_data_source_block           mf439_new
_cod_depositor_comments
'Adding full bibliography for 7047765--7047770.cif.'
_cod_original_cell_volume        2809.37(4)
_cod_database_code               7047765
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Cu2(CH3CN)7(CH2Cl2)3(AlO3C36F46)2
_shelx_estimated_absorpt_t_max   0.536
_shelx_estimated_absorpt_t_min   0.420
_reflns_odcompleteness_completeness 97.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H) groups, All C(H,H,H) groups
2. Restrained distances
 Cl3-C17 = Cl4-C17
 1.771 with sigma of 0.01
 Cl3-Cl4
 2.916 with sigma of 0.03
 Cl4-C17 = Cl3-C17
 1.75 with sigma of 0.01
 Cl4-Cl3
 2.9 with sigma of 0.02
 C1S-Cl1 \\sim C1S-Cl2
 with sigma of 0.02
 N3-C13 \\sim N1-C13A
 with sigma of 0.01
 C14-C13 \\sim C14A-C13A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13A \\sim C13 \\sim C14A \\sim C14: within 1.6A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Cl2 \\sim C1S \\sim Cl1: within 1.8A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Cl4 \\sim C17: within 1.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Cl3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C16) = Uanis(N2)
Uanis(N1) = Uanis(N3)
4. Rigid body (RIGU) restrains
 Cl4, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C13(0.5) C14(0.5) H14D(0.5) H14E(0.5) H14F(0.5) Cu1(0.16667)
 N1(0.5) N2(0.16667) C16(0.16667) H16(0.5) C1S(0.16667) H1SA(0.16667)
 H1SB(0.16667) Cl1(0.16667) Cl2(0.16667) Cu2(0.16667) N3(0.5) C13A(0.5)
 C14A(0.5) H14A(0.5) H14B(0.5) H14C(0.5) Cl3(0.33) Cl4(0.33) C17(0.33)
 H17A(0.33) H17B(0.33)
6.a Everything fixed:
 H16, H1SA, H1SB
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
6.c Idealised Me refined as rotating group:
 C14(H14D,H14E,H14F), C14A(H14A,H14B,H14C)
;
_shelx_res_checksum              57483
_olex2_submission_special_instructions 'No special instructions were received'