An anionic nucleophilic d(4) carbyne complex.
Hill, Anthony F.; Kong, Richard Y.; Chemical communications (Cambridge, England) 53 (2017) 2032–2035; doi:10.1039/c6cc09718a

data_7119547
_publ_section_title
;
 An anionic nucleophilic d(4) carbyne complex.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2032
_journal_page_last               2035
_journal_paper_doi               10.1039/c6cc09718a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C33 H56.03 Br O2 P2 W'
_chemical_formula_sum            'C33 H55 Br O2 P2 W'
_chemical_formula_weight         809.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.561(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8206(5)
_cell_length_b                   14.4920(5)
_cell_length_c                   22.3551(9)
_cell_measurement_reflns_used    6839
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      23.1600
_cell_measurement_theta_min      3.4550
_cell_volume                     3482.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00 -34.00   1.00    1.35    --  -11.07 178.00-120.00   64
  2  \w    -61.00  39.00   1.00    1.35    --   11.30 -57.00   0.00  100
  3  \w    -21.00  87.00   1.00    1.35    --   11.30  77.00 -90.00  108
  4  \w    -17.00  84.00   1.00    1.35    --   11.30  57.00 150.00  101
  5  \w    -39.00  62.00   1.00    1.35    --  -11.07  57.00-150.00  101
  6  \w   -100.00 -35.00   1.00    1.35    --  -11.07-178.00  30.00   65
  7  \w    -17.00  53.00   1.00    1.35    --   11.30  57.00  30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0526290000
_diffrn_orient_matrix_UB_12      -0.0220226000
_diffrn_orient_matrix_UB_13      -0.0098311000
_diffrn_orient_matrix_UB_21      0.0375771000
_diffrn_orient_matrix_UB_22      0.0382949000
_diffrn_orient_matrix_UB_23      0.0101016000
_diffrn_orient_matrix_UB_31      0.0132914000
_diffrn_orient_matrix_UB_32      -0.0210046000
_diffrn_orient_matrix_UB_33      0.0286653000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.975
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51350
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.103
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4465
_reflns_number_total             6134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09718a2.cif
_cod_data_source_block           Compound_5b
_cod_depositor_comments
'Adding full bibliography for 7119543--7119548.cif.'
_cod_database_code               7119547
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C37 H66 O2 P2 W'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C128) = Uanis(C129) = Uanis(C132) = Uanis(C131) = Uanis(C130)
Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32)
3. Others
 Sof(C30)=Sof(H24C)=Sof(C28)=Sof(H27A)=Sof(C32)=Sof(H30D)=Sof(H30C)=Sof(C29)=
 Sof(H31C)=Sof(H31D)=Sof(C31)=Sof(H32C)=Sof(H1BF)=Sof(H1BE)=1-FVAR(1)
 Sof(C130)=Sof(H24A)=Sof(H24B)=Sof(C128)=Sof(H27)=Sof(C132)=Sof(H30A)=
 Sof(H30B)=Sof(C129)=Sof(H31A)=Sof(H31B)=Sof(C131)=Sof(H32A)=Sof(H32B)=
 Sof(H1AC)=Sof(H1AD)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H5), C16(H0AA), C22(H17), C128(H27), C28(H27A)
4.b Secondary CH2 refined with riding coordinates:
 C8(H3B,H3A), C9(H6B,H6A), C27(H3AA,H3AB), C21(H8A,H8B), C12(H10A,H10B),
 C13(H11A,H11B), C14(H2AA,H2AB), C11(H13A,H13B), C17(H14A,H14B), C15(H15A,H15B),
  C20(H16A,H16B), C18(H1AA,H1AB), C24(H19A,H19B), C23(H20A,H20B), C130(H24A,
 H24B), C19(H25A,H25B), C25(H26A,H26B), C26(H28A,H28B), C132(H30A,H30B),
 C129(H31A,H31B), C131(H32A,H32B), C32(H30D,H30C), C29(H31C,H31D), C33(H1AC,
 H1AD), C33(H1BF,H1BE)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H24C), C31(H32C)
4.d Idealised Me refined as rotating group:
 C4(H21A,H21B,H21C), C5(H22A,H22B,H22C), C3(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.748
_oxdiff_exptl_absorpt_empirical_full_min 0.821