Novel Family of Homoleptic Copper(I) Complexes Featuring Disubstituted Cyanamides: Combined Synthetic, Structural, and Theoretical Study
Melekhova, Anna A.; Novikov, Alexander S.; Panikorovsky, Taras L.; Bokach, Nadezhda A.; Kukushkin, Vadim Yu.; New J. Chem. 41 (2017) 14557–14566; doi:10.1039/C7NJ02798B

data_7056685
_publ_section_title
;
 Novel Family of Homoleptic Copper(I) Complexes Featuring Disubstituted
 Cyanamides: Combined Synthetic, Structural, and Theoretical Study
;
_journal_issue                   23
_journal_name_full               'New J. Chem.'
_journal_page_first              14557
_journal_page_last               14566
_journal_paper_doi               10.1039/C7NJ02798B
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'B F4, C24 H40 Cu N8'
_chemical_formula_sum            'C24 H40 B Cu F4 N8'
_chemical_formula_weight         591.00
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-05 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.521(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8710(7)
_cell_length_b                   16.8165(14)
_cell_length_c                   21.3749(14)
_cell_measurement_reflns_used    4681
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.8410
_cell_measurement_theta_min      3.2080
_cell_volume                     2901.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega  -82.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.5593    0.0000   30.0000 127

  2 omega  -87.00  -61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.5593 -178.0000 -150.0000 26

  3 omega  -93.00  -35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.5593  -57.0000   30.0000 58

  4 omega   50.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6531  178.0000  -30.0000 52

  5 omega  -49.00  -23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.5593  -38.0000  -60.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0643510000
_diffrn_orient_matrix_UB_12      -0.0250366000
_diffrn_orient_matrix_UB_13      0.0020325000
_diffrn_orient_matrix_UB_21      -0.0420608000
_diffrn_orient_matrix_UB_22      0.0314473000
_diffrn_orient_matrix_UB_23      0.0150162000
_diffrn_orient_matrix_UB_31      -0.0224090000
_diffrn_orient_matrix_UB_32      0.0128358000
_diffrn_orient_matrix_UB_33      -0.0331009000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15903
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.799
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0429P)^2^+3.1112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5551
_reflns_number_total             6568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02798b2.cif
_cod_data_source_block           3
_cod_database_code               7056685
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30 N5 Cu H10'
_reflns_odcompleteness_completeness 97.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
;
_olex2_submission_special_instructions 'No special instructions were received'