A [C<sub>1</sub> + C<sub>2</sub>] route to propargylidyne complexes.
Hill, Anthony F.; Manzano, Richard A.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6596–6610; doi:10.1039/c9dt00876d

data_7701667
_publ_section_title
;
 A [C<sub>1</sub> + C<sub>2</sub>] route to propargylidyne complexes.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6596
_journal_page_last               6610
_journal_paper_doi               10.1039/c9dt00876d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C30 H31 B Fe N6 O2 W'
_chemical_formula_sum            'C30 H31 B Fe N6 O2 W'
_chemical_formula_weight         758.12
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-18 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.404(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0081(3)
_cell_length_b                   15.9662(5)
_cell_length_c                   18.8514(8)
_cell_measurement_reflns_used    4611
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.7550
_cell_measurement_theta_min      3.6140
_cell_volume                     3009.64(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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_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     29.00  94.00   1.00   18.00    --   35.53-133.00  51.00   65
  2  \w    -34.00 105.00   1.00   18.00    --   35.53   0.00  60.00  139
  3  \w      0.00  28.00   1.00   18.00    --   35.53  92.00 -40.49   28
  4  \w    -32.00  52.00   1.00   18.00    --   35.53 -57.00  30.00   84
  5  \w      9.00 103.00   1.00   18.00    --   35.53  77.00-120.00   94
  6  \w     23.00  89.00   1.00   18.00    --   35.53-125.00-180.00   66
  7  \w     38.00 116.00   1.00   65.00    --  108.00-111.00-120.00   78
  8  \w     40.00  98.00   1.00   65.00    --  108.00 -45.00 -60.00   58
  9  \w     40.00 135.00   1.00   65.00    --  108.00 -77.00  90.00   95
 10  \w     40.00  98.00   1.00   65.00    --  108.00 -45.00  60.00   58
 11  \w     40.00  98.00   1.00   65.00    --  108.00 -45.00-180.00   58
 12  \w     40.00  98.00   1.00   65.00    --  108.00 -45.00   0.00   58
 13  \w     38.00 116.00   1.00   65.00    --  108.00-111.00  60.00   78
 14  \w     40.00  98.00   1.00   65.00    --  108.00 -45.00-120.00   58
 15  \w     91.00 176.00   1.00   65.00    --  108.00  45.00-180.00   85
 16  \w     40.00 135.00   1.00   65.00    --  108.00 -77.00 -90.00   95
 17  \w     38.00  90.00   1.00   65.00    --  108.00 -30.00 150.00   52
 18  \w     39.00 177.00   1.00   65.00    --  108.00   0.00 -30.00  138
 19  \w    -34.00  54.00   1.00   18.00    --   35.53 -38.00-150.00   88
 20  \w     -2.00  24.00   1.00   18.00    --   35.53  96.00  69.29   26
 21  \w      6.00  95.00   1.00   18.00    --   35.53  19.00-150.00   89
 22  \w      9.00 103.00   1.00   18.00    --   35.53  77.00 120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1529072000
_diffrn_orient_matrix_UB_12      0.0014985000
_diffrn_orient_matrix_UB_13      -0.0065726000
_diffrn_orient_matrix_UB_21      -0.0188079000
_diffrn_orient_matrix_UB_22      0.0010095000
_diffrn_orient_matrix_UB_23      -0.0815323000
_diffrn_orient_matrix_UB_31      -0.0021296000
_diffrn_orient_matrix_UB_32      0.0964550000
_diffrn_orient_matrix_UB_33      0.0010137000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0645
_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       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.584
_diffrn_reflns_theta_max         66.584
_diffrn_reflns_theta_min         4.696
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79017
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_recrystallization_method
'Red crystals grown from vapour-vapour diffusion of hexane into a DCM solution'
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.024
_refine_diff_density_max         4.997
_refine_diff_density_min         -3.160
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+109.4603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4533
_reflns_number_total             5301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00876d1.cif
_cod_data_source_block           ram-069_scale
_cod_database_code               7701667
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H31 B1 N6 O2 Fe1 W1'
_chemical_oxdiff_usercomment     'red needle'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(N4) = Uanis(N6)
Uanis(C2) = Uanis(C1)
3.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C27(H27), C7(H7), C11(H11), C17(H17), C8(H8), C10(H10), C14(H14),
 C15(H15), C9(H9), C12(H12), C13(H13)
3.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              80236
_ins_header
;
TITL RAM-069_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.008106  15.966216  18.851428  90.0000  92.4042  90.0000
ZERR    4.00   0.000331   0.000527   0.000752   0.0000   0.0036   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O Fe W
UNIT 120.00 124.00 4.00 24.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id WC3Fc(CO)2(Tp*)
_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 0.849