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_7047768
_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
'C36 H32 Cu2 Mo4 N4 O8 P4, 2(Al C36 F46 O3), C H2 Cl2'
_chemical_formula_sum            'C109 H34 Al2 Cl2 Cu2 F92 Mo4 N4 O14 P4'
_chemical_formula_weight         4130.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-11
_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                 100.4620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.2675(2)
_cell_length_b                   18.77190(10)
_cell_length_c                   25.8322(2)
_cell_measurement_reflns_used    27217
_cell_measurement_temperature    122.9(2)
_cell_measurement_theta_max      75.0150
_cell_measurement_theta_min      3.2840
_cell_volume                     13479.58(16)
_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      122.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.4094
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -116.00 -20.00   0.50    6.00    --  -44.64 -37.00  90.00  192
  2  \w   -118.00 -73.00   0.50    6.00    --  -44.64-125.00 150.00   90
  3  \w     23.00  98.00   0.50    6.00    --   44.64-125.00 -30.00  150
  4  \w     80.00 177.00   0.50   30.00    --  107.00  61.00-120.00  194
  5  \w     80.00 178.00   0.50   30.00    --  107.00  30.00 120.00  196
  6  \w     37.00 134.00   0.50   30.00    --  107.00 -61.00  90.00  194
  7  \w     27.00 178.00   0.50   30.00    --  107.00   0.00  90.00  302
  8  \w   -114.00 -19.00   0.50    6.00    --  -44.64 -57.00-150.00  190
  9  \w   -119.00 -13.00   0.50    6.00    --  -44.64 -77.00 -30.00  212
 10  \w     94.00 135.00   0.50   30.00    --  107.00 125.00 150.00   82
;
_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      -0.0224658000
_diffrn_orient_matrix_UB_12      0.0696372000
_diffrn_orient_matrix_UB_13      -0.0246979000
_diffrn_orient_matrix_UB_21      -0.0506098000
_diffrn_orient_matrix_UB_22      -0.0296649000
_diffrn_orient_matrix_UB_23      0.0011236000
_diffrn_orient_matrix_UB_31      0.0020196000
_diffrn_orient_matrix_UB_32      0.0316529000
_diffrn_orient_matrix_UB_33      0.0554081000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35932
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.479
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.005
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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 light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_description       block
_exptl_crystal_F_000             8008
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.176
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         11993
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0532P)^2^+41.2695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11733
_reflns_number_total             11993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03723j2.cif
_cod_data_source_block           abs282_abs
_cod_depositor_comments
'Adding full bibliography for 7047765--7047770.cif.'
_cod_database_code               7047768
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C54.5H17AlClCuF46Mo2N2O7P2
_chemical_oxdiff_usercomment     'red block'
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.249
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5B-Mo1
 2.3 with sigma of 0.01
 C7B-Mo1
 2.3 with sigma of 0.02
 C3B-Mo1
 2.3 with sigma of 0.02
 C4B-Mo1
 2.3 with sigma of 0.02
 C5B-C3B
 2.2 with sigma of 0.01
 C14B-C11B
 2.2 with sigma of 0.01
 C6B-Mo1
 2.3 with sigma of 0.02
 C7B-C6B
 1.4 with sigma of 0.02
 Mo2-C8B \\sim Mo2-C8A
 with sigma of 0.002
 C7B-C6B \\sim C5B-C6B \\sim C5B-C4B \\sim C3B-C4B \\sim C7B-C3B
 with sigma of 0.01
 C10B-C11B \\sim C12B-C11B \\sim C13B-C12B \\sim C14B-C13B \\sim C14B-C10B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C8B \\sim C8A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
O3B \\sim O3A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C8A \\sim C8B: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C1B \\sim O1B \\sim C6A: within 1.5A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C4A \\sim C3A \\sim C7A \\sim
C6A \\sim C5A: within 1.6A with sigma of 0.01 and sigma for terminal atoms of
0.02
C14B \\sim C13B \\sim C12B \\sim C11B \\sim C14A \\sim C10B \\sim C10A \\sim
C11A \\sim C12A \\sim C13A: within 1.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C2B \\sim O2B \\sim C1A \\sim O1A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O1B, C1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=Sof(C12B)=Sof(H12B)=Sof(C10B)=
 Sof(H10B)=Sof(C8B)=Sof(O3B)=Sof(C11B)=Sof(H11B)=1-FVAR(1)
 Sof(O3A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C8A)=Sof(C14A)=Sof(H14A)=
 Sof(C10A)=Sof(H10A)=Sof(C13A)=Sof(H13A)=FVAR(1)
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=
 Sof(C5B)=Sof(H5B)=Sof(O1B)=Sof(C1B)=Sof(C2B)=Sof(O2B)=1-FVAR(2)
 Sof(O2A)=Sof(C6A)=Sof(H6A)=Sof(C2A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=
 Sof(C7A)=Sof(H7A)=Sof(C3A)=Sof(H3A)=Sof(C1A)=Sof(O1A)=FVAR(2)
 Fixed Sof: H55A(0.5) H55B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B)
6.b Aromatic/amide H refined with riding coordinates:
 C11A(H11A), C12A(H12A), C14A(H14A), C10A(H10A), C13A(H13A), C13B(H13B),
 C14B(H14B), C12B(H12B), C10B(H10B), C6A(H6A), C4A(H4A), C5A(H5A), C7A(H7A),
 C3A(H3A), C6B(H6B), C7B(H7B), C3B(H3B), C4B(H4B), C5B(H5B), C11B(H11B)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              51710
_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 2.010
_oxdiff_exptl_absorpt_empirical_full_min 0.591