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_7047770
_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
'C14 H21 Cu Fe N2 P5, Al C36 F46 O3, 1[CH2Cl2]'
_chemical_formula_sum            'C51 H23 Al Cl2 Cu F46 Fe N2 O3 P5'
_chemical_formula_weight         1957.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-11
_audit_creation_method
;
Olex2 1.2
(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                 92.1269(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.46563(4)
_cell_length_b                   19.19874(6)
_cell_length_c                   30.69781(11)
_cell_measurement_reflns_used    69187
_cell_measurement_temperature    123.1(2)
_cell_measurement_theta_max      65.7050
_cell_measurement_theta_min      4.0540
_cell_volume                     6752.72(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     21.00 106.00   0.50    7.50    --   40.03  57.00-150.00  170
  2  \w     21.00 116.00   0.50    7.50    --   40.03  57.00 -60.00  190
  3  \w      6.00  94.00   0.50    7.50    --   40.03-125.00-180.00  176
  4  \w     -1.00  68.00   0.50    7.50    --   40.03-125.00  90.00  138
  5  \w     78.00 104.00   0.50   23.50    --   93.50  -9.00   9.60   52
  6  \w    138.00 171.00   0.50   23.50    --   93.50  -9.00   9.60   66
  7  \w     24.00  50.00   0.50   23.50    --   93.50 -71.00 -30.85   52
  8  \w     42.00  68.00   0.50   23.50    --   93.50-111.00  60.00   52
  9  \w      7.00  69.00   0.50   23.50    --   93.50  -9.00   9.60  124
 10  \w     60.00 106.00   0.50   23.50    --   93.50  30.00-180.00   92
 11  \w    140.00 168.00   0.50   23.50    --   93.50  30.00-180.00   56
 12  \w     98.00 134.00   0.50   23.50    --   93.50 178.00 -90.00   72
 13  \w     34.00  78.00   0.50   23.50    --   93.50-111.00 -60.00   88
 14  \w     14.00  39.00   0.50   23.50    --   93.50 -30.00 -60.00   50
 15  \w    113.00 151.00   0.50   23.50    --   93.50  30.00  30.00   76
 16  \w     92.00 126.00   0.50   23.50    --   93.50 -65.00 107.36   68
 17  \w    135.00 161.00   0.50   23.50    --   93.50  77.00 -30.00   52
 18  \w     60.00 104.00   0.50   23.50    --   93.50  30.00 -90.00   88
 19  \w     27.00  53.00   0.50   23.50    --   93.50 -45.00 120.00   52
 20  \w     36.00 103.00   0.50   23.50    --   93.50 178.00-180.00  134
 21  \w     75.00 101.00   0.50   23.50    --   93.50  61.00 150.00   52
 22  \w    117.00 170.00   0.50   23.50    --   93.50  61.00 150.00  106
 23  \w     29.00  58.00   0.50   23.50    --   93.50 -95.00  90.00   58
 24  \w     36.00  87.00   0.50   23.50    --   93.50 178.00 -90.00  102
 25  \w     23.00 116.00   0.50   23.50    --   93.50 -61.00-120.00  186
 26  \w     35.00  63.00   0.50   23.50    --   93.50 -95.00  60.00   56
 27  \w    133.00 159.00   0.50   23.50    --   93.50  15.00 150.00   52
 28  \w     81.00 125.00   0.50   23.50    --   93.50  45.00 120.00   88
 29  \w    128.00 153.00   0.50   23.50    --   93.50  45.00 120.00   50
 30  \w     62.00 140.00   0.50   23.50    --   93.50  61.00  30.00  156
 31  \w     92.00 118.00   0.50   23.50    --   93.50  45.00-150.00   52
 32  \w     68.00 126.00   0.50   23.50    --   93.50  77.00 -30.00  116
 33  \w     66.00 147.00   0.50   23.50    --   93.50  30.00-150.00  162
 34  \w     28.00  66.00   0.50   23.50    --   93.50 -95.00-120.00   76
 35  \w     27.00  90.00   0.50   23.50    --   93.50-111.00  30.00  126
 36  \w     30.00  69.00   0.50   23.50    --   93.50 -30.00 -90.00   78
 37  \w     64.00  90.00   0.50   23.50    --   93.50  45.00-150.00   52
 38  \w    137.00 164.00   0.50   23.50    --   93.50  30.00 -90.00   54
 39  \w     16.00  64.00   0.50   23.50    --   93.50 -30.00  60.00   96
 40  \w     77.00 102.00   0.50   23.50    --   93.50  30.00  60.00   50
 41  \w    145.00 173.00   0.50   23.50    --   93.50  30.00  60.00   56
 42  \w     25.00  50.00   0.50   23.50    --   93.50-111.00 -90.00   50
 43  \w     59.00  87.00   0.50   23.50    --   93.50-111.00 -90.00   56
 44  \w     31.00  56.00   0.50   23.50    --   93.50-111.00 -30.00   50
 45  \w     70.00 105.00   0.50   23.50    --   93.50 178.00 150.00   70
 46  \w     27.00  52.00   0.50   23.50    --   93.50 -95.00  30.00   50
 47  \w     44.00  69.00   0.50   23.50    --   93.50 -65.00 107.36   50
 48  \w     66.00  92.00   0.50   23.50    --   93.50  61.00-150.00   52
 49  \w    113.00 139.00   0.50   23.50    --   93.50  61.00-150.00   52
 50  \w     73.00 122.00   0.50   23.50    --   93.50  61.00 -30.00   98
 51  \w     69.00 127.00   0.50   23.50    --   93.50 -71.00 -30.85  116
 52  \w    140.00 171.00   0.50   23.50    --   93.50  30.00   0.00   62
 53  \w     88.00 147.00   0.50   23.50    --   93.50  15.00 -30.00  118
 54  \w     26.00  51.00   0.50   23.50    --   93.50  15.00 150.00   50
 55  \w     78.00 104.00   0.50   23.50    --   93.50 -88.00 -60.45   52
 56  \w     18.00  67.00   0.50   23.50    --   93.50 -30.00   0.00   98
 57  \w    103.00 128.00   0.50   23.50    --   93.50 111.00  90.00   50
 58  \w     43.00  68.00   0.50   23.50    --   93.50 178.00 -30.00   50
 59  \w     77.00 117.00   0.50   23.50    --   93.50  45.00 -60.00   80
 60  \w     90.00 115.00   0.50   23.50    --   93.50 -61.00 -60.00   50
 61  \w     60.00  86.00   0.50   23.50    --   93.50  77.00-150.00   52
 62  \w    145.00 170.00   0.50   23.50    --   93.50  77.00  90.00   50
 63  \w     89.00 114.00   0.50   23.50    --   93.50 -15.00-150.00   50
 64  \w    108.00 133.00   0.50   23.50    --   93.50   0.00-150.00   50
 65  \w     86.00 123.00   0.50   23.50    --   93.50 -87.00 -10.89   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0785539000
_diffrn_orient_matrix_UB_12      0.0649168000
_diffrn_orient_matrix_UB_13      0.0042954000
_diffrn_orient_matrix_UB_21      -0.0270738000
_diffrn_orient_matrix_UB_22      0.0054708000
_diffrn_orient_matrix_UB_23      0.0486574000
_diffrn_orient_matrix_UB_31      0.1057333000
_diffrn_orient_matrix_UB_32      -0.0468371000
_diffrn_orient_matrix_UB_33      0.0116531000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            109308
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.092
_diffrn_reflns_theta_max         66.092
_diffrn_reflns_theta_min         3.688
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.706
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.37b (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_description       block
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         11781
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+5.4884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11618
_reflns_number_total             11781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03723j2.cif
_cod_data_source_block           mf450_mp_abs
_cod_depositor_comments
'Adding full bibliography for 7047765--7047770.cif.'
_cod_database_code               7047770
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H21AlCuF46FeN2O3P5
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.252
_reflns_odcompleteness_completeness 98.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14A-C13A \\sim C13B-C14B \\sim C12A-C11A \\sim C12B-C11B
 with sigma of 0.01
 N1B-C11B \\sim N1A-C11A \\sim N2A-C13A \\sim N2B-C13B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N2A \\sim C13A \\sim C14A \\sim C14B \\sim C13B \\sim N2B \\sim N1B \\sim C11A
\\sim C12A \\sim C12B \\sim C11B \\sim N1A: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C13B)=Sof(N2B)=1-FVAR(1)
 Sof(N2A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
 Sof(N1B)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11B)=1-FVAR(2)
 Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(N1A)=FVAR(2)
5.a Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C),
 C8(H8A,H8B,H8C), C12A(H12A,H12B,H12C), C14A(H14A,H14B,H14C), C14B(H14D,H14E,
 H14F), C12B(H12D,H12E,H12F)
;
_shelx_res_checksum              21281
_shelx_fab_checksum              67998
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.495
_oxdiff_exptl_absorpt_empirical_full_min 0.764