Isolation of a (Dinitrogen)Tricopper(I) Complex
Murray, Leslie J.; Weare, Walter W.; Shearer, Jason; Mitchell, Alyssa D.; Abboud, Khalil A.; Journal of the American Chemical Society  (2014) 140919104426007–; doi:10.1021/ja506445d

data_4122643
_publ_section_title
;
 Isolation of a (Dinitrogen)Tricopper(I) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              140919104426007
_journal_paper_doi               10.1021/ja506445d
_journal_year                    2014
_chemical_formula_moiety         'C45 H63 Cu3 N8, C4 H8 O'
_chemical_formula_sum            'C49 H71 Cu3 N8 O'
_chemical_formula_weight         978.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-07-28 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 109.8086(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.508(2)
_cell_length_b                   11.6305(12)
_cell_length_c                   20.199(2)
_cell_measurement_reflns_used    7040
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     4532.8(8)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0889
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39697
_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         27.500
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.8889
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
; 
 Flack x determined using 3141 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         10409
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0226P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7751
_reflns_number_total             10409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja506445d_si_002.cif
_cod_data_source_block           murr17
_cod_database_code               4122643
_shelx_estimated_absorpt_t_min   0.776
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-3
_shelx_res_checksum              76210
_shelx_hkl_checksum              57191