Spodium bonding in bis(alkynyl)mecurials.
Onn, Chee S.; Hill, Anthony F.; Ward, Jas S.; Chemical communications (Cambridge, England) 60 (2024) 2552–2555; doi:10.1039/d3cc06027f

data_7132792
_publ_section_title
;
 Spodium bonding in bis(alkynyl)mecurials.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2552
_journal_page_last               2555
_journal_paper_doi               10.1039/d3cc06027f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C52 H52 B2 Hg N14 O4 Se2 W2'
_chemical_formula_sum            'C52 H52 B2 Hg N14 O4 Se2 W2'
_chemical_formula_weight         1684.90
_chemical_name_common            'Thesis - Compound 4.6a - CO16'
_chemical_name_systematic        CO16
_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
_audit_creation_date             2020-09-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-21 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                117.984(6)
_cell_angle_beta                 91.487(5)
_cell_angle_gamma                103.840(5)
_cell_formula_units_Z            4
_cell_length_a                   13.7335(9)
_cell_length_b                   21.8752(11)
_cell_length_c                   22.6730(13)
_cell_measurement_reflns_used    5953
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.5630
_cell_measurement_theta_min      3.7520
_cell_volume                     5764.1(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.963
_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    -53.00  18.00   1.00   20.00    --  -36.03  57.00 -90.00   71
  2  \w   -100.00 -17.00   1.00   20.00    --  -36.03 -38.00  30.00   83
  3  \w    -91.00  28.00   1.00   20.00    --  -36.03   0.00-120.00  119
  4  \w     27.00  87.00   1.00   20.00    --   36.03-125.00-150.00   60
  5  \w     27.00  88.00   1.00   20.00    --   36.03-125.00  30.00   61
  6  \w    109.00 172.00   1.00   80.00    --  105.15  45.00 -90.00   63
  7  \w     35.00  85.00   1.00   80.00    --  105.15 -30.00 120.00   50
  8  \w    110.00 173.00   1.00   80.00    --  105.15  77.00   0.00   63
  9  \w     36.00 127.00   1.00   80.00    --  105.15 -30.00  30.00   91
 10  \w     35.00 127.00   1.00   80.00    --  105.15 -30.00 -60.00   92
 11  \w     50.00 109.00   1.00   80.00    --  105.15-111.00  30.00   59
 12  \w     96.00 127.00   1.00   80.00    --  105.15 -30.00 120.00   31
 13  \w     40.00 101.00   1.00   80.00    --  105.15 -95.00 -90.00   61
 14  \w     41.00  98.00   1.00   80.00    --  105.15 -95.00 -30.00   57
 15  \w     41.00 130.00   1.00   80.00    --  105.15 -77.00  30.00   89
 16  \w     44.00 106.00   1.00   80.00    --  105.15 -95.00-180.00   62
 17  \w     35.00 126.00   1.00   80.00    --  105.15 -30.00-150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0916969000
_diffrn_orient_matrix_UB_12      -0.0115491000
_diffrn_orient_matrix_UB_13      0.0351423000
_diffrn_orient_matrix_UB_21      -0.0483278000
_diffrn_orient_matrix_UB_22      -0.0746677000
_diffrn_orient_matrix_UB_23      -0.0623759000
_diffrn_orient_matrix_UB_31      0.0543982000
_diffrn_orient_matrix_UB_32      -0.0348227000
_diffrn_orient_matrix_UB_33      0.0308610000
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.1216
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34266
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.968
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       plate
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.058
_refine_diff_density_max         3.433
_refine_diff_density_min         -2.660
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1411
_refine_ls_number_reflns         21405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0740P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13065
_reflns_number_total             21405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06027f2.cif
_cod_data_source_block           co16_co_wsehg_phen_scale
_cod_database_code               7132792
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H52 B2 Hg N14 O4 Se2 W2'
_chemical_oxdiff_usercomment     'THF pentane vap diff'
_reflns_odcompleteness_completeness 99.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B2A(H2A), B1(H1), B1A(H1A), B2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C45A(H45A), C30(H30), C25(H25), C40A(H40A), C13(H13), C45(H45), C50(H50),
 C40(H40), C50A(H50A), C17A(H17A), C17(H17), C13A(H13A), C22A(H22A), C21(H21),
 C35A(H35A), C11A(H11A), C11(H11), C12(H12), C22(H22), C12A(H12A), C35(H35),
 C19A(H19A), C30A(H30A), C18A(H18A), C21A(H21A), C25A(H25A), C19(H19), C18(H18)
2.c Idealised Me refined as rotating group:
 C47A(H47A,H47B,H47C), C32(H32D,H32E,H32F), C28(H28D,H28E,H28F), C43A(H43A,
 H43B,H43C), C48(H48D,H48E,H48F), C42(H42D,H42E,H42F), C37(H37D,H37E,H37F),
 C48A(H48A,H48B,H48C), C23(H23D,H23E,H23F), C33(H33D,H33E,H33F), C27(H27D,H27E,
 H27F), C43(H43D,H43E,H43F), C33A(H33A,H33B,H33C), C42A(H42A,H42B,H42C),
 C38(H38D,H38E,H38F), C52A(H52A,H52B,H52C), C52(H52D,H52E,H52F), C28A(H28A,H28B,
 H28C), C38A(H38A,H38B,H38C), C37A(H37A,H37B,H37C), C47(H47D,H47E,H47F),
 C23A(H23A,H23B,H23C), C32A(H32A,H32B,H32C), C27A(H27A,H27B,H27C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated for the pentane solvent which was
highly volatile and 27 electrons were found in a volume of 
147 A^3^ in 2 voids per unit cell. This is consistent with the 
presence of 0.167[C5H12] per Asymmetric Unit which account for 
28 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52628
_shelx_hkl_checksum              11795
_shelx_fab_checksum              50371
_ins_header
;
TITL CO_WSeHg_phen_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  13.733478  21.875157  22.673035 117.9841  91.4867 103.8400
ZERR    4.00   0.000856   0.001149   0.001304   0.0056   0.0049   0.0049
LATT  1
SFAC C H B N O Se W Hg
UNIT 208.00 208.00 8.00 56.00 16.00 8.00 8.00 4.00
TREF
HKLF 4
END
;
_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 1.612
_oxdiff_exptl_absorpt_empirical_full_min 0.537