Template synthesis of an intermediate in silver salt metathesis using a calix[4]arene-based diphosphine ligand
Emerson-King, Jack; Chaplin, Adrian B.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00567D

data_7712717
_publ_section_title
;
 Template synthesis of an intermediate in silver salt metathesis using a
 calix[4]arene-based diphosphine ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00567D
_journal_year                    2023
_chemical_formula_moiety         'C156 H156 Cl2 O8 P4 Rh2,0.5(C6 H14)'
_chemical_formula_sum            'C159 H163 Cl2 O8 P4 Rh2'
_chemical_formula_weight         2602.48
_chemical_melting_point          ?
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-03-16 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                75.020(5)
_cell_angle_beta                 87.021(4)
_cell_angle_gamma                89.684(4)
_cell_formula_units_Z            2
_cell_length_a                   17.9994(8)
_cell_length_b                   18.5281(8)
_cell_length_c                   21.3105(14)
_cell_measurement_reflns_used    13670
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.9240
_cell_measurement_theta_min      3.7430
_cell_volume                     6855.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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   -128.00 -35.00   1.00   15.00    --  -40.86-178.00  60.00   93
  2  \w    -68.00  29.00   1.00   15.00    --  -40.86  57.00  90.00   97
  3  \w   -111.00 -14.00   1.00   15.00    --  -40.86 -57.00 -60.00   97
  4  \w      9.00 115.00   1.00   15.00    --   40.86  77.00-150.00  106
  5  \w      1.00  81.00   1.00   15.00    --   40.86 -99.00  90.00   80
  6  \w     57.00 128.00   1.00   15.00    --   40.86 178.00 -30.00   71
  7  \w     25.00 109.00   1.00   60.00    --  106.00 -94.00 -30.00   84
  8  \w     78.00 176.00   1.00   60.00    --  106.00  61.00-120.00   98
  9  \w     25.00 109.00   1.00   60.00    --  106.00 -94.00-150.00   84
 10  \w     31.00 130.00   1.00   60.00    --  106.00 -30.00   0.00   99
 11  \w     36.00 134.00   1.00   60.00    --  106.00 -61.00-120.00   98
 12  \w     34.00 121.00   1.00   60.00    --  106.00-125.00 120.00   87
 13  \w     82.00 177.00   1.00   60.00    --  106.00  45.00  30.00   95
 14  \w     25.00 109.00   1.00   60.00    --  106.00 -94.00 -90.00   84
 15  \w     94.00 178.00   1.00   60.00    --  106.00 125.00 -90.00   84
 16  \w     34.00 121.00   1.00   60.00    --  106.00-125.00-180.00   87
 17  \w     94.00 178.00   1.00   60.00    --  106.00 125.00 -60.00   84
 18  \w     94.00 178.00   1.00   60.00    --  106.00 125.00 -30.00   84
 19  \w     36.00 134.00   1.00   60.00    --  106.00 -61.00   0.00   98
 20  \w   -111.00 -14.00   1.00   15.00    --  -40.86 -57.00  60.00   97
 21  \w   -115.00  -9.00   1.00   15.00    --  -40.86 -77.00  30.00  106
 22  \w   -114.00 -19.00   1.00   15.00    --  -40.86 -37.00 120.00   95
 23  \w   -115.00  -9.00   1.00   15.00    --  -40.86 -77.00 -90.00  106
 24  \w     57.00 128.00   1.00   15.00    --   40.86 178.00  60.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0007952000
_diffrn_orient_matrix_UB_12      0.0384048000
_diffrn_orient_matrix_UB_13      -0.0733613000
_diffrn_orient_matrix_UB_21      -0.0567991000
_diffrn_orient_matrix_UB_22      0.0574544000
_diffrn_orient_matrix_UB_23      0.0133354000
_diffrn_orient_matrix_UB_31      0.0641808000
_diffrn_orient_matrix_UB_32      0.0513134000
_diffrn_orient_matrix_UB_33      0.0074739000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23471
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         6.370
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2730
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-hexane at 293 K'
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.037
_refine_diff_density_max         4.858
_refine_diff_density_min         -1.647
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1595
_refine_ls_number_reflns         23471
_refine_ls_number_restraints     263
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1793
_refine_ls_R_factor_gt           0.1471
_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^)+(0.1526P)^2^+106.8875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3643
_refine_ls_wR_factor_ref         0.3859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16703
_reflns_number_total             23471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00567d2.cif
_cod_data_source_block           0303abc17s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7712717
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(7)
 0.037(4) 0.07(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 O66-C67 \\sim O76-C77 \\sim O96-C97 \\sim O86-C87 \\sim O96A-C97A \\sim
O66A-C67A \\sim O76A-C77A ~
 O86A-C87A
 with sigma of 0.01
 C88A-C87A \\sim C89A-C88A \\sim C79A-C78A \\sim C78A-C77A \\sim C69A-C68A
\\sim C68A-C67A \\sim C99A-
 C98A \\sim C99A-C98B \\sim C98A-C97A \\sim C98B-C97A \\sim C79-C78 \\sim
C78-C77 \\sim C99-C98 \\sim C98-
 C97 \\sim C89-C88 \\sim C88-C87 \\sim C68-C67 \\sim C69-C68
 with sigma of 0.01
 C902-C901 \\sim C903-C902 \\sim C903-C903_$1
 with sigma of 0.01
 C901-C903 \\sim C902-C903_$1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O66 \\sim C67 \\sim C68 \\sim C69 \\sim C97A \\sim C98A \\sim C98B \\sim C99A
\\sim C901 \\sim C901 \\sim C902 \\sim C902 \\sim C903 \\sim C903: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(C901) \\sim Ueq, Uanis(C902) \\sim Ueq, Uanis(C903) \\sim Ueq,
Uanis(C903) \\sim Ueq, Uanis(C902) \\sim Ueq, Uanis(C901) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H97A(0.5) H97B(0.5) H97C(0.5) H97D(0.5) C98A(0.5) H98A(0.5)
 H98B(0.5) C98B(0.5) H98C(0.5) H98D(0.5) H99A(0.5) H99B(0.5) H99C(0.5)
 H99D(0.5) H99E(0.5) H99F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C33(H33C,H33D), C53(H53C,H53D), C67(H67C,H67D), C68(H68C,H68D), C77(H77C,
 H77D), C78(H78C,H78D), C87(H87C,H87D), C88(H88C,H88D), C97(H97E,H97F),
 C98(H98E,H98F), C607(H60A,H60B), C708(H70B,H70C), C809(H80A,H80B), C906(H90B,
 H90C), C33A(H33A,H33B), C53A(H53A,H53B), C67A(H67A,H67B), C68A(H68A,H68B),
 C77A(H77A,H77B), C78A(H78A,H78B), C87A(H87A,H87B), C88A(H88A,H88B), C97A(H97A,
 H97B), C97A(H97C,H97D), C98A(H98A,H98B), C98B(H98C,H98D), C617(H61B,H61C),
 C718(H71B,H71C), C819(H81B,H81C), C916(H91B,H91C), C902(H90G,H90H), C903(H90I,
 H90J)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C61(H61), C65(H65), C70(H70),
  C71(H71), C75(H75), C81(H81), C85(H85), C90(H90), C91(H91), C95(H95),
 C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C11A(H11A), C12A(H12A), C13A(H13A),
 C14A(H14A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A),
 C28A(H28A), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A), C48A(H48A), C49A(H49A),
 C50A(H50A), C51A(H51A), C52A(H52A), C61A(H61A), C65A(H65A), C70A(H70A),
 C71A(H71A), C75A(H75A), C81A(H81A), C85A(H85A), C90A(H90A), C91A(H91A),
 C95A(H95A)
6.c Idealised Me refined with riding coordinates:
 C99A(H99A,H99B,H99C), C99A(H99D,H99E,H99F)
6.d Idealised Me refined as rotating group:
 C69(H69D,H69E,H69F), C79(H79D,H79E,H79F), C89(H89D,H89E,H89F), C99(H99G,H99H,
 H99I), C69A(H69A,H69B,H69C), C79A(H79A,H79B,H79C), C89A(H89A,H89B,H89C),
 C901(H90D,H90E,H90F)
;
_shelx_res_checksum              45486
_shelx_hkl_checksum              22825
_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 10.408
_oxdiff_exptl_absorpt_empirical_full_min 0.458