Well-defined coinage metal transfer agents for the synthesis of NHC-based nickel, rhodium and palladium macrocycles.
Andrew, Rhiann E.; Storey, Caroline M.; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8937–8944; doi:10.1039/c6dt01263a

data_7039210
_publ_section_title
;
 Well-defined coinage metal transfer agents for the synthesis of NHC-based
 nickel, rhodium and palladium macrocycles.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8937
_journal_page_last               8944
_journal_paper_doi               10.1039/c6dt01263a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C50 H70 Br4 Cu4 N10'
_chemical_formula_sum            'C50 H70 Br4 Cu4 N10'
_chemical_formula_weight         1384.96
_chemical_melting_point          ?
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-24 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                100.004(2)
_cell_angle_beta                 96.750(2)
_cell_angle_gamma                106.179(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2779(2)
_cell_length_b                   10.9565(3)
_cell_length_c                   15.7732(5)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.6760
_cell_measurement_theta_min      2.9530
_cell_volume                     1332.04(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -3.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   38.0000    0.0000 102

  2 omega   35.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  178.0000  120.0000 78

  3 omega  -10.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   77.0000 -150.0000 112

  4 omega   35.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  178.0000 -180.0000 78

  5 omega -114.00  -57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590 -178.0000   60.0000 57

  6 omega -101.00    9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  -77.0000  -90.0000 110

  7 omega -107.00  -81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590 -178.0000  -60.0000 26

  8 omega -106.00    5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  -19.0000  -90.0000 111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0588700000
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_diffrn_orient_matrix_UB_13      -0.0117386000
_diffrn_orient_matrix_UB_21      -0.0413451000
_diffrn_orient_matrix_UB_22      0.0153421000
_diffrn_orient_matrix_UB_23      0.0354872000
_diffrn_orient_matrix_UB_31      -0.0551169000
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_diffrn_orient_matrix_UB_33      -0.0274628000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.100
_diffrn_reflns_theta_max         27.100
_diffrn_reflns_theta_min         2.957
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-pentane at 293 K'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0294P)^2^+0.6463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4916
_reflns_number_total             5863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01263a2.cif
_cod_data_source_block           0156abc15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039209--7039212.cif.
;
_cod_original_cell_volume        1332.03(6)
_cod_database_code               7039210
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C22(H22A,H22B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C20(H20), C21(H21), C26(H26), C27(H27)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'