Isolable acetylene complexes of copper and silver
Noonikara-Poyil, Anurag; Ridlen, Shawn G.; Fernández, Israel; Dias, H. V. Rasika; Chemical Science 13 (2022) 7190–7203; doi:10.1039/D2SC02377F

data_1567003
_publ_section_title
;
 Isolable acetylene complexes of copper and silver
;
_journal_issue                   24
_journal_name_full               'Chemical Science'
_journal_page_first              7190
_journal_page_last               7203
_journal_paper_doi               10.1039/D2SC02377F
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C17 H6 B Cu F18 N6, C14 H16'
_chemical_formula_sum            'C31 H22 B Cu F18 N6'
_chemical_formula_weight         894.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-02-22 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.989(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0640(5)
_cell_length_b                   13.6074(6)
_cell_length_c                   11.4278(5)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      32.30
_cell_measurement_theta_min      2.37
_cell_volume                     1719.44(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Photon II 7 CPAD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest Photon II 7'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_detector       'Photon II 7 CPAD'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30468
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.029
_diffrn_reflns_theta_min         2.519
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'KFF MO-2KC-90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0026(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6197
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0341P)^2^+4.5455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4610
_reflns_number_total             6197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02377f3.cif
_cod_data_source_block           hrd36_0m_a
_cod_depositor_comments
'Adding full bibliography for 1567002--1567006.cif.'
_cod_database_code               1567003
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.819
_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. Restrained distances
 C19-C1A
 1.51 with sigma of 0.02
 C1A-C1B = C1A-C1F = C1C-C1D
 1.39 with sigma of 0.02
 C1B-C1C = C1D-C1E = C1E-C1F
 1.38 with sigma of 0.02
 C1A-C1C
 2.42 with sigma of 0.04
 C1B-C1D
 2.39 with sigma of 0.04
 C1A-C1E
 2.41 with sigma of 0.04
 C1C-C1E = C1D-C1F
 2.4 with sigma of 0.04
 C19-C1B = C19-C1F
 2.52 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1A
 with sigma of 0.02
 C1A-C1E \\sim C1A-C1C \\sim C1F-C1D \\sim C1B-C1F \\sim C1C-C1E \\sim C1B-C1D
 with sigma of 0.04
 C19-C1F \\sim C19-C1B
 with sigma of 0.04
3. Restrained planarity
 C19, C1A, C1B, C1C, C1D, C1E, C1F
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C19 \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
5. Rigid body (RIGU) restrains
 C19, C1A, C1B, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) C1A(0.5) C1B(0.5) H1B(0.5) C1C(0.5) H1C(0.5) C1D(0.5) H1D(0.5)
 C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5)
7.a Ternary CH refined with riding coordinates:
 B(H)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C13(H13), C14(H14), C17(H17), C15(H15), C16(H16), C11(H11),
 C1B(H1B), C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F)
7.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              6599
_shelx_hkl_checksum              12483
_olex2_submission_special_instructions 'No special instructions were received'