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_7045227
_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         'C25 H37 B N6 O2 Si W'
_chemical_formula_sum            'C25 H37 B N6 O2 Si W'
_chemical_formula_weight         676.35
_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                 109.839(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6360(4)
_cell_length_b                   14.8272(5)
_cell_length_c                   16.3046(6)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.3350
_cell_measurement_theta_min      3.6660
_cell_volume                     2873.47(18)
_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):'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\f snd \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0571374000
_diffrn_orient_matrix_UB_12      0.0014086000
_diffrn_orient_matrix_UB_13      -0.0275790000
_diffrn_orient_matrix_UB_21      0.0065613000
_diffrn_orient_matrix_UB_22      0.0457943000
_diffrn_orient_matrix_UB_23      -0.0098798000
_diffrn_orient_matrix_UB_31      0.0159980000
_diffrn_orient_matrix_UB_32      -0.0136877000
_diffrn_orient_matrix_UB_33      -0.0358000000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45892
_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         26.371
_diffrn_reflns_theta_min         3.239
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44164
_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    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method
'Crystal were grown from a solution of pentane stored at -20 degrees Celcius.'
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.531
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0124P)^2^+11.8427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4665
_reflns_number_total             5868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04576j5.cif
_cod_data_source_block           ram-011_scale1
_cod_depositor_comments
'Adding full bibliography for 7045226--7045228.cif.'
_cod_database_code               7045227
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C25 H37 B1 N6 O2 Si W'
_chemical_oxdiff_usercomment     'orange needle'
_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:
 C12(H12), C17(H17), C22(H22)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              26867
_ins_header
'TITL RAM-011_scale1 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 12.635960 14.827168 16.304606 90.0000 109.8394 90.0000 ZERR 4.00 0.000422 0.000469 0.000557 0.0000 0.0038 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H B N O Si W UNIT 100.00 148.00 4.00 24.00 8.00 4.00 4.00 TREF HKLF 4 END'
_olex2_submission_original_sample_id Tp*(CO)2WCC(Me)C(SiMe3)Me
_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 1.777
_oxdiff_exptl_absorpt_empirical_full_min 0.727