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_7047767
_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         'C8 H12 Cu N4, Al C16 F36 O4, C2 H3 N'
_chemical_formula_sum            'C26 H15 Al Cu F36 N5 O4'
_chemical_formula_weight         1235.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.61200(10)
_cell_length_b                   17.1552(2)
_cell_length_c                   23.7300(3)
_cell_measurement_reflns_used    9041
_cell_measurement_temperature    122.95(18)
_cell_measurement_theta_max      75.3080
_cell_measurement_theta_min      4.5490
_cell_volume                     4320.07(8)
_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_environment      N~2~
_diffrn_ambient_temperature      122.95(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.965
_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    -58.00  24.00   1.00    2.00    --  -45.40  37.00 150.00   82
  2  \w      3.00  84.00   1.00    2.00    --   45.40 -99.00  30.00   81
  3  \w     33.00 143.00   1.00    8.00    --  107.00 -15.00-120.00  110
  4  \w     90.00 178.00   1.00    8.00    --  107.00  77.00  60.00   88
  5  \w     34.00 130.00   1.00    8.00    --  107.00 -30.00  60.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0841146000
_diffrn_orient_matrix_UB_12      -0.0646334000
_diffrn_orient_matrix_UB_13      0.0247339000
_diffrn_orient_matrix_UB_21      0.0505802000
_diffrn_orient_matrix_UB_22      -0.0575780000
_diffrn_orient_matrix_UB_23      -0.0443534000
_diffrn_orient_matrix_UB_31      0.1070896000
_diffrn_orient_matrix_UB_32      -0.0236521000
_diffrn_orient_matrix_UB_33      0.0404543000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13779
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.333
_diffrn_reflns_theta_min         3.179
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.548
_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 colourless'
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 3242 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     990
_refine_ls_number_reflns         8404
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0495P)^2^+0.1164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                7937
_reflns_number_total             8404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03723j2.cif
_cod_data_source_block           op_abs_det_ana
_cod_depositor_comments
'Adding full bibliography for 7047765--7047770.cif.'
_cod_database_code               7047767
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CuC8H12N4AlO4C16F46C2H3N
_chemical_oxdiff_usercomment     'colorless block'
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.532
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F17B-F16B \\sim F16B-F18B \\sim F18B-F17B
 with sigma of 0.01
 F14B-F15B \\sim F15B-F13B \\sim F13B-F14B
 with sigma of 0.02
 F13B-C17B \\sim F15B-C17B \\sim F14B-C17B \\sim F14A-C17A \\sim F13A-C17A
\\sim F15A-C17A
 with sigma of 0.01
 F27B-F26B \\sim F26B-F25B \\sim F25B-F27B
 with sigma of 0.02
 F25B-C22B \\sim F26B-C22B \\sim F27B-C22B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F18B \\sim F17B: within 1.4A with sigma of 0.01 and sigma for terminal atoms of
0.02
F12A \\sim F10B \\sim F17B \\sim F18A \\sim F16B \\sim F16A \\sim F14B \\sim
F14A: within 1.1A with sigma of 0.01 and sigma for terminal atoms of 0.02
F16A \\sim F16B: within 1A with sigma of 0.005 and sigma for terminal atoms of
0.01
C16B \\sim C16A \\sim C18B \\sim C18A \\sim C17B \\sim C17A: within 1.4A with
sigma of 0.005 and sigma for terminal atoms of 0.04
F19B \\sim F19A: within 1A with sigma of 0.02 and sigma for terminal atoms of
0.04
F36B \\sim F28A: within 1.2A with sigma of 0.01 and sigma for terminal atoms of
0.02
F15B \\sim C17B: within 1.5A with sigma of 0.01 and sigma for terminal atoms of
0.02
C22A \\sim C22B: within 1.1A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(F35B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F27B)=Sof(C22B)=Sof(F26B)=Sof(F25B)=Sof(F19B)=Sof(C20B)=Sof(F21B)=
 Sof(F20B)=Sof(C21B)=Sof(F22B)=Sof(F24B)=Sof(F23B)=1-FVAR(1)
 Sof(F24A)=Sof(F20A)=Sof(F25A)=Sof(F19A)=Sof(F23A)=Sof(F27A)=Sof(F26A)=
 Sof(F21A)=Sof(F22A)=Sof(C22A)=Sof(C20A)=Sof(C21A)=FVAR(1)
 Sof(F17B)=Sof(C18B)=Sof(F16B)=Sof(F18B)=Sof(F11B)=Sof(F10B)=Sof(C16B)=
 Sof(F12B)=Sof(C17B)=Sof(F14B)=Sof(F15B)=Sof(F13B)=1-FVAR(2)
 Sof(F12A)=Sof(F15A)=Sof(F18A)=Sof(F14A)=Sof(F16A)=Sof(F11A)=Sof(F10A)=
 Sof(F13A)=Sof(F17A)=Sof(C17A)=Sof(C18A)=Sof(C16A)=FVAR(2)
 Sof(F34B)=Sof(C26B)=Sof(F36B)=Sof(F35B)=Sof(C24B)=Sof(F28B)=Sof(F29B)=
 Sof(F30B)=Sof(F31B)=Sof(F32B)=Sof(F33B)=Sof(C25B)=1-FVAR(3)
 Sof(F31A)=Sof(F30A)=Sof(F34A)=Sof(F36A)=Sof(F33A)=Sof(F29A)=Sof(F32A)=
 Sof(F28A)=Sof(F35A)=Sof(C25A)=Sof(C26A)=Sof(C24A)=FVAR(3)
5.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C),
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              82498
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.640