Metal-Ligand Covalency Enables Room Temperature Molecular Qubit Candidates
Fataftah, Majed S.; Krzyaniak, Matthew D.; Vlaisavljevich, Bess; Wasielewski, Michael R.; Zadrozny, Joseph; Freedman, Danna; Chemical Science  (2019) –; doi:10.1039/C9SC00074G

data_1551191
_publ_section_title
;
 Metal-Ligand Covalency Enables Room Temperature Molecular Qubit
 Candidates
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00074G
_journal_year                    2019
_chemical_formula_moiety         'C12 H8 Cu Se4, 2(C24 H20 P)'
_chemical_formula_sum            'C60 H48 Cu P2 Se4'
_chemical_formula_weight         1210.30
_chemical_name_systematic
'tetraphenyl phosphonium copper bis(diselenocatecholate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc210dfx
_audit_creation_date             2018-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-05 deposited with the CCDC.    2019-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.517(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1972(9)
_cell_length_b                   15.0275(12)
_cell_length_c                   15.2359(12)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    250.04
_cell_measurement_theta_max      29.89
_cell_measurement_theta_min      2.57
_cell_volume                     2555.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250.04
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68791
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.606
_diffrn_reflns_theta_min         1.906
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.378
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1127 before and 0.0622 after correction. The Ratio of minimum to maximum transmission is 0.6559. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_preparation
'In DMF, with two equivalents of selenocatechol and 1 equivalent of CuCl2 with NBu4OH and Ph4PBr'
_exptl_crystal_recrystallization_method
'Layered DMF solution of the compound under Et2O at -35 C'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0028(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         7855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0303P)^2^+1.9123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6612
_reflns_number_total             7855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00074g2.cif
_cod_data_source_block           msf6_49_3
_cod_database_code               1551191
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C007(H007), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G),
 C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M),
 C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S),
 C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y)
;
_shelx_res_checksum              7781
_olex2_exptl_crystal_mounting_method 'Mounted under paratone'
_olex2_submission_original_sample_id 'Compound 4'
_olex2_submission_special_instructions 'No special instructions were received'