Coordination chemistry of phosphinocarbynes: phosphorus vs. carbyne site selectivity.
Colebatch, Annie L.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4355–4365; doi:10.1039/c6dt04770j

data_7042314
_publ_section_title
;
 Coordination chemistry of phosphinocarbynes: phosphorus vs. carbyne site
 selectivity.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4355
_journal_page_last               4365
_journal_paper_doi               10.1039/c6dt04770j
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C42 H49 Au1 B2 Cl1 N12 O4 P1 W2, C4 H10 O'
_chemical_formula_sum            'C46 H59 Au B2 Cl N12 O5 P W2'
_chemical_formula_weight         1512.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-11-20 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                66.723(7)
_cell_angle_beta                 69.805(7)
_cell_angle_gamma                73.373(9)
_cell_formula_units_Z            2
_cell_length_a                   12.5001(13)
_cell_length_b                   14.7647(14)
_cell_length_c                   17.4599(10)
_cell_measurement_reflns_used    3130
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2735.9(5)
_computing_cell_refinement       'CrysAlis, (Agilent Technologies, 2013)'
_computing_data_collection       'Xcalibur, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis, (Agilent Technologies, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Agilent Technologies Xcalibur'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20633
_diffrn_reflns_theta_full        25.115
_diffrn_reflns_theta_max         28.540
_diffrn_reflns_theta_min         1.763
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.001
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Agilent Technologies, 2013)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.072
_refine_diff_density_max         11.22
_refine_diff_density_min         -6.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9965
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9625
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.0019174
_refine_ls_shift/su_mean         0.0000917
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.474E+04 0.404E+04 0.217E+04 0.110E+04 -321. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1747
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1747
_reflns_limit_h_max              16
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              -16
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5382
_reflns_number_total             11228
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      0.16
_oxford_refine_ls_r_factor_ref   0.1542
_oxford_refine_ls_scale          2.154(14)
_oxford_reflns_number_all        9625
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c6dt04770j1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7042309--7042314.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C46 H59 Au1 B2 Cl1 N12 O5 P1 W2'
_cod_database_code               7042314
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
REM CONT EXTPARAM 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.01 = C(35) TO C(34) 
U(IJ) 0.0, 0.01 = C(1) TO P(1) 
U(IJ) 0.0, 0.01 = C(2) TO O(2) 
U(IJ) 0.0, 0.01 = C(5) TO O(5) 
U(IJ) 0.0, 0.01 = C(43) TO C(42) 
U(IJ) 0.0, 0.01 = N(31) TO N(32) 
VIBR 0.0, 0.01 = C(71) TO C(72), C(72) TO C(73) 
VIBR 0.0, 0.01 = C(72) TO C(73), C(73) TO C(74) 
VIBR 0.0, 0.01 = C(73) TO C(74), C(74) TO C(75) 
VIBR 0.0, 0.01 = C(74) TO C(75), C(75) TO C(76) 
VIBR 0.0, 0.01 = C(75) TO C(76), C(76) TO C(77) 
VIBR 0.0, 0.01 = C(76) TO C(71), C(71) TO C(78) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;