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_7047766
_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
'C28 H20 Cu Mo4 O8 P4, Al C36 F46 O3, 1[CH2Cl2], 1[CH2Cl2]'
_chemical_formula_sum            'C66 H24 Al Cl4 Cu F46 Mo4 O11 P4'
_chemical_formula_weight         2606.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-12
_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                111.280(2)
_cell_angle_beta                 95.785(2)
_cell_angle_gamma                96.565(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2007(3)
_cell_length_b                   18.7374(4)
_cell_length_c                   21.9873(6)
_cell_measurement_reflns_used    14716
_cell_measurement_temperature    123.0(10)
_cell_measurement_theta_max      32.1520
_cell_measurement_theta_min      3.5130
_cell_volume                     4220.9(2)
_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_temperature      123.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5096
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.865
_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   -109.00 -35.00   1.00  250.00    --  -18.71-178.00  90.00   74
  2  \w    -20.00  28.00   1.00  250.00    --   19.65  96.00 -67.00   48
  3  \w    -54.00  49.00   1.00  250.00    --   19.65 -57.00 -30.00  103
  4  \w    -59.00  53.00   1.00  250.00    --   19.65 -77.00  90.00  112
;
_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      0.0277908000
_diffrn_orient_matrix_UB_12      0.0212330000
_diffrn_orient_matrix_UB_13      -0.0172115000
_diffrn_orient_matrix_UB_21      -0.0039562000
_diffrn_orient_matrix_UB_22      -0.0349070000
_diffrn_orient_matrix_UB_23      -0.0279224000
_diffrn_orient_matrix_UB_31      -0.0580835000
_diffrn_orient_matrix_UB_32      0.0050930000
_diffrn_orient_matrix_UB_33      -0.0123145000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41468
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.603
_diffrn_reflns_theta_min         3.500
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.827
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.530
_refine_diff_density_min         -2.018
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         26612
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18298
_reflns_number_total             26612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03723j2.cif
_cod_data_source_block           abs249_ap_abs
_cod_depositor_comments
'Adding full bibliography for 7047765--7047770.cif.'
_cod_database_code               7047766
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AlC65Cl2CuF46H22Mo4O11P4
_chemical_oxdiff_usercomment     'red-orange block'
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.745
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C5B \\sim C6B \\sim C4B \\sim C3B \\sim C7B \\sim O2A: within 1.6A with sigma
of 0.02 and sigma for terminal atoms of 0.02
3. Others
 Sof(C5B)=Sof(H5B)=Sof(C7B)=Sof(H7B)=Sof(C2B)=Sof(C6B)=Sof(H6B)=Sof(C4B)=
 Sof(H4B)=Sof(C3B)=Sof(H3B)=Sof(O2B)=1-FVAR(1)
 Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C6A)=Sof(H6A)=Sof(C3A)=Sof(H3A)=
 Sof(C7A)=Sof(H7A)=Sof(C2A)=Sof(O2A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C26(H26), C24(H24), C27(H27), C25(H25), C21(H21), C17(H17),
 C18(H18), C19(H19), C20(H20), C11(H11), C14(H14), C13(H13), C10(H10), C12(H12),
  C5A(H5A), C5B(H5B), C7B(H7B), C4A(H4A), C6A(H6A), C3A(H3A), C7A(H7A),
 C6B(H6B), C4B(H4B), C3B(H3B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 184.0 electrons were 
found in a volume of 697.0\%A^3 in 3 voids. 
This is consistent with the presence of 
1[CH2Cl2], 1[CH2Cl2] per formula unit 
which account for 168.0 electrons.
;
_shelx_res_checksum              62863
_shelx_fab_checksum              91770
_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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.907