An unexpected transmetalation intermediate: isolation and structural characterization of a solely CH3 bridged di-copper(i) complex.
Molteni, Roberto; Bertermann, Rüdiger; Edkins, Katharina; Steffen, Andreas; Chemical communications (Cambridge, England) 52 (2016) 5019–5022; doi:10.1039/c6cc01510g

data_7118916
_publ_section_title
;
 An unexpected transmetalation intermediate: isolation and structural
 characterization of a solely CH3 bridged di-copper(i) complex.
;
_journal_issue                   28
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5019
_journal_page_last               5022
_journal_paper_doi               10.1039/c6cc01510g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C38 H36 Cu2 P2'
_chemical_formula_sum            'C38 H36 Cu2 P2'
_chemical_formula_weight         681.75
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2015-10-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-09 deposited with the CCDC.
2016-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                97.647(1)
_cell_angle_beta                 94.311(1)
_cell_angle_gamma                95.342(1)
_cell_formula_units_Z            2
_cell_length_a                   10.0317(3)
_cell_length_b                   12.1017(4)
_cell_length_c                   13.3609(4)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.458
_cell_volume                     1594.30(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24518
_diffrn_reflns_theta_full        25.9975
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  0.9329
_exptl_absorpt_correction_T_min  0.7380
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0341 before and 0.0308 after correction.
The Ratio of minimum to maximum transmission is 0.7911.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4200
_exptl_crystal_description       prism
_exptl_crystal_F_000             705.9452
_exptl_crystal_preparation       'cut from larger prism'
_exptl_crystal_size_max          0.595
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.4719
_refine_diff_density_min         -0.5334
_refine_diff_density_rms         0.1047
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             13.1898
_refine_ls_goodness_of_fit_ref   1.0486
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6267
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0484
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.7017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5660
_reflns_number_total             6267
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cc01510g2.cif
_cod_data_source_block           13S021
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 7118916.cif.
;
_cod_database_code               7118916
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-H2c \\sim C2-H2b \\sim C2-H2a
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C11(H11), C4(H4), C30(H30), C32(H32), C35(H35), C36(H36), C37(H37),
 C10(H10), C17(H17), C22(H22), C24(H24), C12(H12), C5(H5), C13(H13), C25(H25),
 C19(H19), C29(H29), C23(H23), C20(H20), C7(H7), C26(H26), C28(H28), C31(H31),
 C34(H34), C18(H18), C38(H38), C8(H8), C14(H14), C6(H6)
3.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perflourotether oil'
_olex2_submission_special_instructions 'No special instructions were received'