Symmetric and Non-symmetric Anthracen-diyl Bis(alkylidynes)
Hill, Anthony; Frogley, Benjamin; Welsh, Steven S.; Dalton Transactions  (2021) –; doi:10.1039/D1DT02537F

data_7708366
_publ_section_title
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 Symmetric and Non-symmetric Anthracen-diyl Bis(alkylidynes)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02537F
_journal_year                    2021
_chemical_formula_moiety         'C58 H48 B2 Br2 N12 O4 Pd S6 W2'
_chemical_formula_sum            'C58 H48 B2 Br2 N12 O4 Pd S6 W2'
_chemical_formula_weight         1824.98
_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
_audit_creation_date             2021-04-13
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
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_audit_update_record
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2021-04-21 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                85.74(3)
_cell_angle_beta                 70.68(3)
_cell_angle_gamma                69.06(3)
_cell_formula_units_Z            2
_cell_length_a                   16.076(3)
_cell_length_b                   16.868(3)
_cell_length_c                   18.561(4)
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_cell_measurement_theta_max      24.03
_cell_measurement_theta_min      2.2
_cell_volume                     4431(2)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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_temperature      100.0(2)
_diffrn_detector_area_resol_mean 13.3
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.730
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.710762
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_unetI/netI     0.1173
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.730
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77608
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.730
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.172
_diffrn_reflns_theta_min         1.164
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    3.874
_exptl_absorpt_correction_T_max  0.4345
_exptl_absorpt_correction_T_min  0.1505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       needle
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.08
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_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.309
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.1091
_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^)+(0.1869P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2793
_refine_ls_wR_factor_ref         0.3226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9078
_reflns_number_total             22760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02537f2.cif
_cod_data_source_block           Compound_3b
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4430.5(19)
_cod_database_code               7708366
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3.a Ternary CH refined with riding coordinates:
 B2(H2), B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C23(H23), C15(H15), C53(H53), C24(H24), C54(H54), C30(H30),
 C32(H32), C16(H16), C25(H25), C14(H14), C49(H49), C37(H37), C38(H38), C41(H41),
  C13(H13), C26(H26), C6(H6), C31(H31), C58(H58), C45(H45), C50(H50), C44(H44),
 C42(H42), C7(H7), C8(H8), C57(H57), C9(H9)
3.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C), C48(H48A,H48B,
 H48C), C46(H46A,H46B,H46C), C40(H40A,H40B,H40C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12997
_shelx_hkl_checksum              45840
_shelx_fab_checksum              15684
_olex2_submission_special_instructions 'No special instructions were received'