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_7056686
_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, C20 H32 Cu N8 O4'
_chemical_formula_sum            'C20 H32 B Cu F4 N8 O4'
_chemical_formula_weight         598.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.906(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8926(2)
_cell_length_b                   17.9661(3)
_cell_length_c                   15.0570(2)
_cell_measurement_reflns_used    12600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3345
_cell_measurement_theta_min      2.7416
_cell_volume                     2674.62(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -48.00  -23.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4031   38.0000  -90.0000 25

  2 omega  -80.00  -35.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4031 -178.0000  -60.0000 45

  3 omega    8.00   86.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968   57.0000 -120.0000 78

  4 omega   26.00   95.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968   57.0000   30.0000 69

  5 omega   32.00  100.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968 -178.0000 -150.0000 68

  6 omega   60.00   99.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968    0.0000   30.0000 39

  7 omega  -42.00   71.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968  -19.0000 -150.0000 113

  8 omega  -28.00    1.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968    0.0000   30.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0026163000
_diffrn_orient_matrix_UB_12      0.0193774000
_diffrn_orient_matrix_UB_13      0.0409455000
_diffrn_orient_matrix_UB_21      0.0578206000
_diffrn_orient_matrix_UB_22      0.0209021000
_diffrn_orient_matrix_UB_23      -0.0112047000
_diffrn_orient_matrix_UB_31      -0.0424026000
_diffrn_orient_matrix_UB_32      0.0273121000
_diffrn_orient_matrix_UB_33      -0.0204784000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24671
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.493(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         12292
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0327P)^2^+0.6195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11785
_reflns_number_total             12292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02798b2.cif
_cod_data_source_block           4
_cod_database_code               7056686
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu N2 O2 C15 H20'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.507(7)
 0.493(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B),
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B)
;
_olex2_submission_special_instructions 'No special instructions were received'