Synthesis and Reactivity of Dinuclear Copper(I) Pyridine, Diimine Complexes
Stephan, Michel; Dammannn, Wiebke; Burger, Peter; Dalton Transactions  (2022) –; doi:10.1039/D2DT02307E

data_7710976
_publ_section_title
;
 Synthesis and Reactivity of Dinuclear Copper(I) Pyridine, Diimine
 Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02307E
_journal_year                    2022
_chemical_formula_moiety         'C48 H66 Cl Cu2 N6, Cl2 Cu, C H2 Cl2'
_chemical_formula_sum            'C49 H68 Cl5 Cu3 N6'
_chemical_formula_weight         1108.96
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2c80nb
_audit_creation_date             2021-11-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.4530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.448(2)
_cell_length_b                   11.4613(9)
_cell_length_c                   37.179(3)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.16
_cell_volume                     10500.7(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_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  0.0696
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            160292
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.860
_diffrn_reflns_theta_min         1.112
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1097 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.8746. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       bar
_exptl_crystal_F_000             4608
_exptl_crystal_recrystallization_method 'DCM/n-hexane diffusion'
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1195
_refine_ls_number_reflns         25824
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+10.7358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18206
_reflns_number_total             25824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02307e2.cif
_cod_data_source_block           ms_25_1
_cod_database_code               7710976
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cu4-Cl4 \\sim Cu3-Cl3 \\sim Cu4-Cl5 \\sim Cu3-Cl2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cu4 \\sim Cl4 \\sim Cl3 \\sim Cu3 \\sim Cl5 \\sim Cl2: within 1.7A with sigma
of 0.001 and sigma for terminal atoms of 0.001 within 1.7A
4. Others
 Sof(Cl4)=Sof(Cu4)=Sof(Cl5)=1-FVAR(1)
 Sof(Cu3)=Sof(Cl2)=Sof(Cl3)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C01T(H01E,H01F), C02I(H02F,H02G), C024(H02Z,H), C027(H02,HA), C01O(H01K,H01L),
  C01U(H01M,H01O), C01V(H01P,H01R), C02G(H3,HD), C03H(H18,H28), C03F(H19,H29)
5.b Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C01C(H01C), C01J(H01J), C01N(H01N), C01S(H01S), C01W(H01W),
 C02A(H02A), C02C(H02C), C013(H013), C020(H020), C01B(H01G), C01F(H01H),
 C01I(H01I), C01Q(H01Q), C02D(H1), C02J(H4), C02S(H9), C022(H022), C023(H023),
 C026(H026)
5.c Idealised Me refined as rotating group:
 C01P(H01A,H01B,H01D), C02E(H02B,H02D,H02E), C02M(H02H,H02I,H02J), C02R(H02K,
 H02L,H02M), C02U(H02N,H02O,H02P), C02X(H02Q,H02R,H02S), C02Y(H02T,H02U,H02V),
 C02Z(H02W,H02X,H02Y), C03C(H03A,H03B,H03C), C03D(H03D,H03E,H03F), C03E(H03G,
 H03H,H03I), C031(H03J,H03K,H03L), C032(H03M,H03N,H03O), C035(H03P,H03Q,H03R),
 C037(H03S,H03T,H03U), C038(H03V,H03W,H03X), C02F(H2,HB,HC), C02L(H5,HE,HF),
 C02N(H6,HG,HH), C02O(H7,HI,HJ), C02P(H8,HK,HL), C02T(H10,HM,HN), C02V(H11,HO,
 HP), C03A(H03Y,HQ,HR), C03B(H03Z,HS,HT), C03G(H03,HU,HV), C03I(H12,HW,HX),
 C029(H13,HY,HZ), C033(H14,H20,H21), C034(H15,H22,H23), C036(H16,H24,H25),
 C039(H17,H26,H27)
;
_olex2_submission_special_instructions 'No special instructions were received'