Synthesis and Reactivity of New Copper(I) Hydride Dimers
Jordan, Abraham J.; Wyss, Chelsea M.; Bacsa, John; Sadighi, Joseph P.; Organometallics 35 (2016) 613–; doi:10.1021/acs.organomet.6b00025

data_4088367
_publ_section_title
;
 Synthesis and Reactivity of New Copper(I) Hydride Dimers
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              613
_journal_paper_doi               10.1021/acs.organomet.6b00025
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C36 H48 Cu N3'
_chemical_formula_sum            'C36 H48 Cu N3'
_chemical_formula_weight         586.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-07
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.08.05 svn.r3207 for OlexSys, GUI svn.r5081)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.200(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5381(13)
_cell_length_b                   19.114(2)
_cell_length_c                   16.3664(19)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.595
_cell_measurement_theta_min      2.473
_cell_volume                     3270.6(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.632
_diffrn_reflns_theta_min         1.646
_diffrn_source                   'sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1026 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.8665.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of toluene and pentane by vapor diffusion'
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.224
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         9194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+3.1498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7470
_reflns_number_total             9194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00025_si_002.cif
_cod_data_source_block           aj-2-46
_cod_database_code               4088367
_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.a Ternary CH refined with riding coordinates:
 C23(H23), C8(H8), C26(H26), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C14(H14A,H14B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C21(H21), C6(H6), C5(H5), C19(H19), C20(H20), C29(H29), C34(H34),
 C32(H32), C35(H35), C33(H33), C36(H36)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              82261
_shelx_hkl_checksum              1360
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id AJ-2-46
_olex2_submission_special_instructions 'No special instructions were received'