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_7047769
_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 C16 F36 O4, 1(C H2 Cl2)'
_chemical_formula_sum            'C31 H23 Al Cl2 Cu F36 Fe N2 O4 P5'
_chemical_formula_weight         1543.63
_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             2018-07-12
_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                90
_cell_angle_beta                 98.166(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9037(3)
_cell_length_b                   27.5664(6)
_cell_length_c                   17.8993(3)
_cell_measurement_reflns_used    17852
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.6670
_cell_measurement_theta_min      3.8660
_cell_volume                     5325.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.877
_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    -97.00   9.00   0.25   20.00    --  -19.91 -38.00-180.00  424
  2  \w   -101.00  15.00   0.25   20.00    --  -19.91 -77.00 -60.00  464
  3  \w   -110.00 -32.00   0.25   20.00    --  -19.91 178.00 -30.00  312
  4  \w    -49.00  58.00   0.25   20.00    --  -19.91  38.00 -60.00  428
  5  \w     -4.00  21.00   0.25   20.00    --   21.47 -99.00-180.00  100
;
_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      -0.0025898000
_diffrn_orient_matrix_UB_12      0.0256802000
_diffrn_orient_matrix_UB_13      -0.0023733000
_diffrn_orient_matrix_UB_21      0.0378251000
_diffrn_orient_matrix_UB_22      0.0017036000
_diffrn_orient_matrix_UB_23      0.0355591000
_diffrn_orient_matrix_UB_31      0.0536780000
_diffrn_orient_matrix_UB_32      0.0000333000
_diffrn_orient_matrix_UB_33      -0.0182153000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55908
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.321
_diffrn_reflns_theta_min         3.227
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.925
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.225
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1515
_refine_ls_number_reflns         16663
_refine_ls_number_restraints     2709
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0441P)^2^+3.3963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13655
_reflns_number_total             16663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03723j2.cif
_cod_data_source_block           mp_abs_ana
_cod_depositor_comments
'Adding full bibliography for 7047765--7047770.cif.'
_cod_database_code               7047769
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C31H23AlCl2CuF36FeN2O4P5
_chemical_oxdiff_usercomment     'gruener Block'
_reflns_odcompleteness_completeness 97.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F20A-C25 \\sim F19B-C25 \\sim F19A-C25 \\sim F21B-C25 \\sim F20B-C25 \\sim
F21A-C25
 with sigma of 0.01
 C17A-C16 \\sim C18C-C16 \\sim C16-C19C \\sim C19B-C16 \\sim C18A-C16 \\sim
C17B-C16 \\sim C18B-C16 ~
 C17C-C16 \\sim C19A-C16
 with sigma of 0.01
 C23A-C20A \\sim C23B-C20B \\sim C21A-C20A \\sim C20B-C21B \\sim C22B-C20B
\\sim C22A-C20A
 with sigma of 0.01
 C20C-C23C \\sim C20C-C22C \\sim C20C-C21C
 with sigma of 0.02
 C23C-C22C \\sim C22C-C21C \\sim C23C-C21C
 with sigma of 0.04
 F18C-C23C \\sim F16C-C23C \\sim F17C-C23C \\sim F14C-C22C \\sim F15C-C22C
\\sim F13C-C22C \\sim F11C-
 C21C \\sim F12C-C21C \\sim F10C-C21C
 with sigma of 0.02
 F18C-F16C \\sim F16C-F17C \\sim F17C-F18C \\sim F14C-F15C \\sim F15C-F13C
\\sim F13C-F14C \\sim F11C-
 F12C \\sim F12C-F10C \\sim F10C-F11C
 with sigma of 0.02
 F18C-C20C \\sim F16C-C20C \\sim F17C-C20C \\sim F14C-C20C \\sim F15C-C20C
\\sim F13C-C20C \\sim F11C-
 C20C \\sim F12C-C20C \\sim F10C-C20C
 with sigma of 0.1
 F12A-F10A \\sim F10A-F11A \\sim F11A-F12A
 with sigma of 0.02
 F17B-F18B \\sim F18B-F16B \\sim F16B-F17B
 with sigma of 0.01
 O2B-C20B \\sim O2C-C20C \\sim O2A-C20A
 with sigma of 0.02
 F11A-C21A \\sim F10B-C21B \\sim F10A-C21A \\sim F12B-C21B \\sim F11B-C21B
\\sim F12A-C21A \\sim F14B-
 C22B \\sim F15A-C22A \\sim F13A-C22A \\sim F13B-C22B \\sim F15B-C22B \\sim
F14A-C22A \\sim F16A-C23A ~
 F18A-C23A \\sim F16B-C23B \\sim F18B-C23B \\sim F17B-C23B \\sim F17A-C23A
 with sigma of 0.01
 F18A-F17A \\sim F17A-F16A \\sim F16A-F18A
 with sigma of 0.02
 Cl1A-C15A \\sim Cl2C-C15C \\sim Cl2A-C15A \\sim Cl1C-C15C \\sim Cl2B-C15B
\\sim Cl1B-C15B
 with sigma of 0.02
 F8A-C19A \\sim F1C-C17C \\sim F4B-C18B \\sim F9A-C19A \\sim F5B-C18B \\sim
F6B-C18B \\sim F7A-C19A ~
 F3C-C17C \\sim F2C-C17C \\sim F3B-C17B \\sim F1B-C17B \\sim F2B-C17B \\sim
F4A-C18A \\sim F8C-C19C ~
 F6A-C18A \\sim F5A-C18A \\sim F9C-C19C \\sim F7C-C19C \\sim F9B-C19B \\sim
F8B-C19B \\sim F7B-C19B ~
 F4C-C18C \\sim F3A-C17A \\sim F6C-C18C \\sim F5C-C18C \\sim F1A-C17A \\sim
F2A-C17A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3B \\sim O3A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
F13A \\sim F12A \\sim F14A \\sim F10A \\sim F15A \\sim C20A \\sim F18A \\sim
F17A \\sim F11A \\sim F16A \\sim C22A \\sim C23A \\sim C21A \\sim F13B \\sim
C22B \\sim F15B \\sim F14B \\sim C20B \\sim C23B \\sim F17B \\sim F18B \\sim
F16B \\sim F10B \\sim C21B \\sim F12B \\sim F11B \\sim O2C \\sim O2A \\sim C20C
\\sim C23C \\sim F18C \\sim F16C \\sim F17C \\sim C22C \\sim F14C \\sim F15C
\\sim F13C \\sim C21C \\sim F11C \\sim F12C \\sim F10C: within 1.6A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Cl1C \\sim Cl2B \\sim Cl2A \\sim C15B \\sim C15C \\sim C15A \\sim Cl1B \\sim
Cl1A \\sim Cl2C: within 1.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
F27A \\sim F21A \\sim F25A \\sim F19A \\sim F26A \\sim F20A \\sim F22A \\sim
F23A \\sim F24A \\sim C24 \\sim C25 \\sim C27A \\sim C26A \\sim F24B \\sim C26B
\\sim F22B \\sim F23B \\sim F25B \\sim C27B \\sim F26B \\sim F27B \\sim F19B
\\sim F20B \\sim F21B: within 1.6A with sigma of 0.01 and sigma for terminal
atoms of 0.02
F1B \\sim F3B \\sim F6A \\sim F2B \\sim F8C \\sim F5A \\sim F4A \\sim F9C \\sim
F9B \\sim F7C \\sim F8B \\sim F3A \\sim F6C \\sim F5C \\sim F2A \\sim F7B \\sim
F1A \\sim F4C \\sim F5B \\sim F9A \\sim F4B \\sim F8A \\sim F6B \\sim F7A \\sim
F2C \\sim F1C \\sim F3C \\sim C17C \\sim C19A \\sim C18B \\sim C17B \\sim C18A
\\sim C19C \\sim C19B \\sim C17A \\sim C18C: within 1.6A with sigma of 0.005
and sigma for terminal atoms of 0.02
F35B \\sim F33A \\sim F34A \\sim F28B \\sim C29B \\sim F35A \\sim C31A \\sim
F29B \\sim F30B \\sim F36A \\sim F36B \\sim F31A \\sim C31B \\sim C30A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F16B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
4. Others
 Sof(F25B)=Sof(C27B)=Sof(F26B)=Sof(F27B)=1-FVAR(1)
 Sof(F27A)=Sof(F25A)=Sof(F26A)=Sof(C27A)=FVAR(1)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=1-FVAR(2)
 Sof(F21A)=Sof(F19A)=Sof(F20A)=FVAR(2)
 Sof(O1B)=1-FVAR(3)
 Sof(O1A)=FVAR(3)
 Sof(O4B)=Sof(F31B)=Sof(C30B)=Sof(F33B)=Sof(F32B)=Sof(F34B)=Sof(C31B)=
 Sof(F36B)=Sof(F35B)=Sof(F30B)=Sof(C29B)=Sof(F28B)=Sof(F29B)=1-FVAR(4)
 Sof(F32A)=Sof(F31A)=Sof(F28A)=Sof(F36A)=Sof(F29A)=Sof(F34A)=Sof(F35A)=
 Sof(F30A)=Sof(F33A)=Sof(O4A)=Sof(C31A)=Sof(C30A)=Sof(C29A)=FVAR(4)
 Fixed Sof: F7A(0.45) O3A(0.75) F13A(0.17) F12A(0.17) F14A(0.17) F10A(0.17)
 F15A(0.17) O2B(0.13) F22A(0.75) C20A(0.17) F18A(0.17) F23A(0.75) F17A(0.17)
 F24A(0.75) F11A(0.17) F16A(0.17) C22A(0.17) C23A(0.17) C19A(0.45) C21A(0.17)
 F8A(0.45) C26A(0.75) F3A(0.45) F1A(0.45) F2A(0.45) C17A(0.45) F4A(0.45)
 F5A(0.45) F6A(0.45) C18A(0.45) F9A(0.45) F2B(0.3) F3B(0.3) F1B(0.3) C17B(0.3)
 C19B(0.3) F8B(0.3) F9B(0.3) F5B(0.3) F4B(0.3) F6B(0.3) C18B(0.3) F7B(0.3)
 F9C(0.25) F7C(0.25) F8C(0.25) C19C(0.25) F4C(0.25) F5C(0.25) F6C(0.25)
 C18C(0.25) F3C(0.25) F2C(0.25) F1C(0.25) C17C(0.25) O3B(0.25) F24B(0.25)
 C26B(0.25) F22B(0.25) F23B(0.25) Cl1A(0.52) Cl2A(0.52) C15A(0.52) H15A(0.52)
 H15B(0.52) Cl1B(0.28) Cl2B(0.28) C15B(0.28) H15C(0.28) H15D(0.28) Cl1C(0.2)
 Cl2C(0.2) C15C(0.2) H15E(0.2) H15F(0.2) F13B(0.13) C22B(0.13) F15B(0.13)
 F14B(0.13) O2A(0.17) C20B(0.13) C23B(0.13) F17B(0.13) F18B(0.13) F16B(0.13)
 F10B(0.13) C21B(0.13) F12B(0.13) F11B(0.13) O2C(0.7) C20C(0.7) C23C(0.7)
 F18C(0.7) F16C(0.7) F17C(0.7) C22C(0.7) F14C(0.7) F15C(0.7) F13C(0.7)
 C21C(0.7) F11C(0.7) F12C(0.7) F10C(0.7)
5.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C15B(H15C,H15D), C15C(H15E,H15F)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              46752
_olex2_diffrn_ambient_temperature_device 123(1)
_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 1.049
_oxdiff_exptl_absorpt_empirical_full_min 0.936