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_7045226
_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         'C24 H35 B N6 O2 Si W'
_chemical_formula_sum            'C24 H35 B N6 O2 Si W'
_chemical_formula_weight         662.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-06-22
_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                90
_cell_angle_beta                 89.668(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3555(3)
_cell_length_b                   14.6772(3)
_cell_length_c                   20.6011(4)
_cell_measurement_reflns_used    9208
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.6070
_cell_measurement_theta_min      3.9040
_cell_volume                     2828.74(12)
_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    'ShelXT (Sheldrick, 2015)'
_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    -37.00  53.00   1.00    2.85    --  -11.22  57.00   0.00   90
  2  \w    -23.00  17.00   1.00    2.85    --  -11.22 -57.00-150.00   40
  3  \w    -45.00  -4.00   1.00    2.85    --  -11.22 -37.00   0.00   41
  4  \w    -85.00 -58.00   1.00    2.85    --  -11.22 -37.00-120.00   27
  5  \w    -74.00 -30.00   1.00    2.85    --  -11.22 -37.00-180.00   44
  6  \w    -13.00  23.00   1.00    2.85    --  -11.22 -99.00-180.00   36
  7  \w     34.00  97.00   1.00    2.85    --   11.30-178.00-120.00   63
  8  \w    -60.00 -35.00   1.00    2.85    --  -11.22-178.00 -90.00   25
;
_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      -0.0722237000
_diffrn_orient_matrix_UB_12      -0.0115292000
_diffrn_orient_matrix_UB_13      0.0067042000
_diffrn_orient_matrix_UB_21      -0.0185764000
_diffrn_orient_matrix_UB_22      0.0468465000
_diffrn_orient_matrix_UB_23      -0.0004186000
_diffrn_orient_matrix_UB_31      -0.0136106000
_diffrn_orient_matrix_UB_32      -0.0028597000
_diffrn_orient_matrix_UB_33      -0.0337728000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26641
_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         3.245
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86642
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.638
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0184P)^2^+3.9723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4629
_reflns_number_total             5791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04576j5.cif
_cod_data_source_block           ram-010_scale1
_cod_depositor_comments
'Adding full bibliography for 7045226--7045228.cif.'
_cod_database_code               7045226
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C24 H35 B1 N6 O23 Si1 W1'
_chemical_oxdiff_usercomment     'Red crystal plate'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C16(H16), C21(H21)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              16763
_ins_header
;
TITL RAM-010_scale1 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073   9.355493  14.677229  20.601089  90.0000  89.6678  90.0000
ZERR    3.00   0.000274   0.000346   0.000405   0.0000   0.0020   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Si W
UNIT 72.00 105.00 3.00 18.00 69.00 3.00 3.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id RAM-010
_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 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.870