Synthesis and reactivity of an anionic allenylidene complex.
Hill, Anthony F.; Manzano, Richard A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1412–1416; doi:10.1039/c7dt04576j

data_7045228
_publ_section_title
;
 Synthesis and reactivity of an anionic allenylidene complex.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1412
_journal_page_last               1416
_journal_paper_doi               10.1039/c7dt04576j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C48 H68 B2 N12 O4 Si2 W2, C5 H12'
_chemical_formula_sum            'C53 H80 B2 N12 O4 Si2 W2'
_chemical_formula_weight         1394.79
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-01
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-11-24 deposited with the CCDC.
2018-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                91.059(2)
_cell_angle_beta                 98.161(2)
_cell_angle_gamma                108.441(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0937(3)
_cell_length_b                   13.1532(3)
_cell_length_c                   22.7516(4)
_cell_measurement_reflns_used    24054
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4600
_cell_measurement_theta_min      3.5660
_cell_volume                     3110.38(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_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    -36.00  63.00   1.00   12.50    --  -11.22  37.00 -30.00   99
  2  \w    -20.00  30.00   1.00   12.50    --  -11.22 -99.00  60.00   50
  3  \w   -100.00 -35.00   1.00   12.50    --  -11.22-178.00  90.00   65
  4  \w    -86.00  13.00   1.00   12.50    --  -11.22 -37.00 -30.00   99
  5  \w    -86.00  13.00   1.00   12.50    --  -11.22 -37.00   0.00   99
  6  \w     34.00  98.00   1.00   12.50    --   11.30-178.00 -60.00   64
  7  \w   -100.00 -35.00   1.00   12.50    --  -11.22-178.00 -30.00   65
  8  \w    -17.00  57.00   1.00   12.50    --   11.30  57.00 -90.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0390575000
_diffrn_orient_matrix_UB_12      0.0336275000
_diffrn_orient_matrix_UB_13      -0.0007453000
_diffrn_orient_matrix_UB_21      -0.0474002000
_diffrn_orient_matrix_UB_22      -0.0406542000
_diffrn_orient_matrix_UB_23      0.0118675000
_diffrn_orient_matrix_UB_31      0.0297193000
_diffrn_orient_matrix_UB_32      0.0215079000
_diffrn_orient_matrix_UB_33      0.0292416000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.267
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.396
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         12726
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+6.5219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10868
_reflns_number_total             12726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04576j5.cif
_cod_data_source_block           ram-23scale_sq
_cod_depositor_comments
'Adding full bibliography for 7045226--7045228.cif.'
_cod_database_code               7045228
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C53 H80 B2 N2 O4 Si2 W2'
_chemical_oxdiff_usercomment
'Grown from DCM/pentane diffusion - Orange crystals'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C202-C201 = C202-C203 = C203-C204
 1.5 with sigma of 0.02
 C200-C201
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C7, C8, C9, C107, C108, C109
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C200, C201, C202, C203, C204
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C107 \\sim C108 \\sim C109: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C200 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C108) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C107) = Uanis(C108) = Uanis(C8)
5. Rigid body (RIGU) restrains
 C7, C8, C9, C107, C108, C109
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C109)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C107)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C108)=Sof(H10G)=Sof(H10H)=Sof(H10I)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C202(H8BA,H8BB), C201(H0CA,H0CB), C203(H4CA,H4CB)
7.b Aromatic/amide H refined with riding coordinates:
 C6BA(H6BA), C0AA(H0AA), C16(H16), C11(H11), C21(H21), C1CA(H1CA)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C7AA(H7AA,H7AB,H7AC), C2AA(H2AA,H2AB,H2AC), C5AA(H5AA,H5AB,
 H5AC), C6AA(H6AA,H6AB,H6AC), C8AA(H8AA,H8AB,H8AC), C23(H23A,H23B,H23C),
 C3BA(H3BA,H3BB,H3BC), C1BA(H1BA,H1BB,H1BC), C18(H18A,H18B,H18C), C2BA(H2BA,
 H2BB,H2BC), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C),
 C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C2CA(H2CA,H2CB,H2CC), C7CA(H7CA,H7CB,H7CC), C109(H10A,H10B,H10C), C107(H10D,
 H10E,H10F), C108(H10G,H10H,H10I), C200(H9BA,H9BB,H9BC), C204(H3CA,H3CB,H3CC)
;
_shelx_res_checksum              80219
_shelx_fab_checksum              30363
_ins_header
;
TITL RAM-23scale in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  11.093745  13.153162  22.751564  91.0590  98.1609 108.4408
ZERR    2.00   0.000265   0.000317   0.000358   0.0016   0.0016   0.0021
LATT  1
SFAC C H B N O Si W
UNIT 106.00 160.00 4.00 4.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.825