Synthesis and reactivity of 9,10-bis(4-trimethylsilylethynylbuta-1,3-diynyl)anthracene derived chromophores
Hill, Anthony; Frogley, Benjamin; Dalton Transactions  (2023) –; doi:10.1039/D3DT00147D

data_7712504
_publ_section_title
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 Synthesis and reactivity of
 9,10-bis(4-trimethylsilylethynylbuta-1,3-diynyl)anthracene derived
 chromophores
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00147D
_journal_year                    2023
_chemical_formula_sum            'C77 H71 N3 Ni2 P4'
_chemical_formula_weight         1281.68
_chemical_name_common            Ni2(m-dppm)2(m-CN-Xylyl)(m-CN-Xylyl)2
_chemical_name_systematic
;
(\m~2~-Xylylisocianide)bis(Xylylisocianide)
(bis(\m~2~-bis(diphenylphosphino)
methane)-di-nickel
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc7s0yy
_audit_creation_method           SHELXL-97
_audit_update_record
;
2004-02-16 deposited with the CCDC.	2023-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.6950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.4008(16)
_cell_length_b                   12.9100(10)
_cell_length_c                   23.6900(18)
_cell_measurement_temperature    100(2)
_cell_volume                     6269.3(8)
_computing_cell_refinement       'SAINT PLUS'
_computing_data_collection       'SAINT PLUS'
_computing_data_reduction        'SAINT PLUS'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25948
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.9153
_exptl_absorpt_correction_T_min  0.5849
_exptl_absorpt_correction_type   empiric
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'deep brown'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rombohedric
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00000(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          11.145
_refine_ls_shift/su_mean         0.055
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+9.7863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                6146
_reflns_number_total             7066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt00147d2.cif
_cod_data_source_block           8
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_cell_measurement_temperature' value '-173(2)' was changed
to '100(2)' -- it was converted from degrees Celsius (C) to kelvins
(K).

data item '_diffrn_ambient_temperature' value '-173(2)' was changed
to '100(2)' -- it was converted from degrees Celsius (C) to kelvins
(K).

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7712504