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_7701670
_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         'C38 H37 B Ge N6 O2 W, C H Cl3'
_chemical_formula_sum            'C39 H38 B Cl3 Ge N6 O2 W'
_chemical_formula_weight         996.35
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-14
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-02-15 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9977(2)
_cell_length_b                   12.82720(10)
_cell_length_c                   19.7393(2)
_cell_measurement_reflns_used    29820
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.7150
_cell_measurement_theta_min      4.1170
_cell_volume                     4032.77(7)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 1.000
_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     -3.00  38.00   1.00    2.50    --   37.04 -57.00 -30.00   41

  2  \w      6.00  40.00   1.00    2.50    --   37.04 -57.00 -60.00   34

  3  \w     44.00  71.00   1.00    2.50    --   37.04 -99.00   0.00   27

  4  \w     43.00  89.00   1.00    2.50    --   37.04-125.00   0.00   46

  5  \w     54.00  83.00   1.00    2.50    --   37.04-125.00  90.00   29

  6  \w     29.00  82.00   1.00    2.50    --   37.04-125.00 -30.00   53

  7  \w     49.00  89.00   1.00    2.50    --   37.04-125.00 -90.00   40

  8  \w     83.00 109.00   1.00   10.00    --  111.00 -77.00 -60.00   26

  9  \w    115.00 141.00   1.00   10.00    --  111.00 -92.00 -90.00   26

 10  \w    112.00 138.00   1.00   10.00    --  111.00 -77.00-150.00   26

 11  \w    121.00 146.00   1.00   10.00    --  111.00 -92.00-150.00   25

 12  \w    102.00 136.00   1.00   10.00    --  111.00 -25.00-150.00   34

 13  \w     86.00 124.00   1.00   10.00    --  111.00 -38.00 -90.00   38

 14  \w     87.00 126.00   1.00   10.00    --  111.00 -46.00-162.59   39

 15  \w     75.00 109.00   1.00   10.00    --  111.00-111.00 -90.00   34

 16  \w     91.00 116.00   1.00   10.00    --  111.00-111.00 -30.00   25

 17  \w     81.00 116.00   1.00   10.00    --  111.00-111.00  60.00   35

 18  \w     84.00 113.00   1.00   10.00    --  111.00-111.00 120.00   29

 19  \w     87.00 113.00   1.00   10.00    --  111.00 -77.00  60.00   26

 20  \w    103.00 130.00   1.00   10.00    --  111.00 -64.00  60.00   27

 21  \w     85.00 114.00   1.00   10.00    --  111.00 -50.00  30.00   29

 22  \w     76.00 112.00   1.00   10.00    --  111.00 -38.00  60.00   36

 23  \w     73.00 119.00   1.00   10.00    --  111.00 -64.00  30.00   46

 24  \w     73.00 116.00   1.00   10.00    --  111.00-111.00  90.00   43

 25  \w     75.00 100.00   1.00   10.00    --  111.00-111.00 150.00   25

 26  \w     73.00 105.00   1.00   10.00    --  111.00 -77.00 150.00   32

 27  \w     57.00  93.00   1.00   10.00    --  111.00 -50.00 120.00   36

 28  \w     46.00  71.00   1.00   10.00    --  111.00 -77.00  60.00   25

 29  \w     63.00 116.00   1.00   10.00    --  111.00-111.00  30.00   53

 30  \w     63.00  91.00   1.00   10.00    --  111.00 -38.00   0.00   28

 31  \w     66.00 131.00   1.00   10.00    --  111.00 -64.00 -60.00   65

 32  \w     65.00 113.00   1.00   10.00    --  111.00-111.00 -60.00   48

 33  \w     63.00  92.00   1.00   10.00    --  111.00 -77.00-150.00   29

 34  \w     62.00 114.00   1.00   10.00    --  111.00-111.00-180.00   52

 35  \w     56.00 116.00   1.00   10.00    --  111.00-111.00-120.00   60

 36  \w     50.00  80.00   1.00   10.00    --  111.00 -92.00 -90.00   30

 37  \w     46.00  88.00   1.00   10.00    --  111.00 -50.00 -60.00   42

 38  \w     47.00  73.00   1.00   10.00    --  111.00 -38.00 -90.00   26

 39  \w     44.00  95.00   1.00   10.00    --  111.00 -50.00-120.00   51

 40  \w     56.00 145.00   1.00   10.00    --  111.00 -12.00-180.00   89

 41  \w    150.00 177.00   1.00   10.00    --  111.00  50.00 -90.00   27

 42  \w    147.00 172.00   1.00   10.00    --  111.00 111.00 -90.00   25

 43  \w    128.00 176.00   1.00   10.00    --  111.00  77.00-180.00   48

 44  \w    110.00 136.00   1.00   10.00    --  111.00  77.00 -60.00   26

 45  \w     97.00 124.00   1.00   10.00    --  111.00  64.00 -60.00   27

 46  \w     92.00 126.00   1.00   10.00    --  111.00  38.00   0.00   34

 47  \w    137.00 163.00   1.00   10.00    --  111.00  38.00  30.00   26

 48  \w    125.00 174.00   1.00   10.00    --  111.00  77.00  30.00   49

 49  \w    129.00 176.00   1.00   10.00    --  111.00  25.00 150.00   47

 50  \w    107.00 133.00   1.00   10.00    --  111.00  25.00  30.00   26

 51  \w     93.00 127.00   1.00   10.00    --  111.00  38.00  30.00   34

 52  \w     90.00 118.00   1.00   10.00    --  111.00  77.00  30.00   28

 53  \w     87.00 112.00   1.00   10.00    --  111.00  25.00 150.00   25

 54  \w     42.00 135.00   1.00   10.00    --  111.00 -25.00  90.00   93

 55  \w     79.00 104.00   1.00    2.50    --   37.04  38.00  90.00   25

 56  \w     41.00 149.00   1.00   10.00    --  111.00 -14.00 -27.32  108

 57  \w     94.00 142.00   1.00   10.00    --  111.00  50.00 -90.00   48

 58  \w     69.00  99.00   1.00    2.50    --   37.04  57.00 -90.00   30

 59  \w     66.00 101.00   1.00    2.50    --   37.04  57.00-150.00   35

 60  \w     41.00  75.00   1.00    2.50    --   37.04  57.00-180.00   34

 61  \w     22.00 104.00   1.00    2.50    --   37.04  57.00-120.00   82

 62  \w     44.00  87.00   1.00   10.00    --  111.00 -50.00-180.00   43

 63  \w     69.00 141.00   1.00   10.00    --  111.00  12.00 -90.00   72

 64  \w     42.00  67.00   1.00   10.00    --  111.00-111.00 -90.00   25

 65  \w     47.00  94.00   1.00   10.00    --  111.00 -92.00-150.00   47

 66  \w     46.00  73.00   1.00   10.00    --  111.00 -77.00-180.00   27

 67  \w     48.00  80.00   1.00   10.00    --  111.00 -25.00-150.00   32

 68  \w     21.00  65.00   1.00    2.50    --   37.04  57.00-150.00   44

 69  \w     22.00  48.00   1.00    2.50    --   37.04  57.00 -90.00   26

 70  \w    -30.00  21.00   1.00    2.50    --   37.04 -57.00  60.00   51

 71  \w     25.00  84.00   1.00    2.50    --   37.04-125.00 150.00   59

 72  \w     42.00  67.00   1.00   10.00    --  111.00-111.00 150.00   25

 73  \w     20.00  57.00   1.00    2.50    --   37.04  38.00  90.00   37

 74  \w     -1.00  32.00   1.00    2.50    --  -37.04  38.00 120.00   33

 75  \w    -66.00 -41.00   1.00    2.50    --  -37.04 -57.00  30.00   25

 76  \w    -34.00  61.00   1.00    2.50    --   37.04 -19.00 -90.00   95

 77  \w    -48.00   0.00   1.00    2.50    --  -37.04  57.00-180.00   48

 78  \w    -65.00 -40.00   1.00    2.50    --  -37.04 -38.00-180.00   25

 79  \w    112.00 137.00   1.00   10.00    --  111.00 178.00-180.00   25

 80  \w    118.00 144.00   1.00   10.00    --  111.00 178.00  30.00   26
;
_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      -0.0961683000
_diffrn_orient_matrix_UB_12      0.0103029000
_diffrn_orient_matrix_UB_13      -0.0021221000
_diffrn_orient_matrix_UB_21      0.0102588000
_diffrn_orient_matrix_UB_22      0.1086404000
_diffrn_orient_matrix_UB_23      0.0330319000
_diffrn_orient_matrix_UB_31      -0.0024841000
_diffrn_orient_matrix_UB_32      0.0501378000
_diffrn_orient_matrix_UB_33      -0.0710552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.885
_diffrn_reflns_theta_min         4.116
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66225
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'Crystals were grown from slow evaporation of a ethanol/chloroform solution at 0 degrees celcius.'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.843
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8148
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0627P)^2^+6.7078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7495
_reflns_number_total             8148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00876d1.cif
_cod_data_source_block           ram-43_scale
_cod_database_code               7701670
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C38 H36 B1 Ge1 N6 O2 W1'
_chemical_oxdiff_usercomment
'Crystals grown from chloroform/ethanol evaporation at 0 degrees celcius'
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.292
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Restrained distances
 Cl2-C100
 1.75 with sigma of 0.02
 Cl3-C100 = Cl1-C100 = Cl2-C100
 1.75 with sigma of 0.02
 Cl6-C200 = Cl5-C200
 1.75 with sigma of 0.02
3. Others
 Fixed Sof: Cl3(0.5) Cl2(0.5) Cl5(0.5) Cl6(0.5) Cl1(0.5) Cl4(0.5) C100(0.5)
 H100(0.5) C200(0.5) H200(0.5)
4.a Ternary CH refined with riding coordinates:
 C100(H100), C200(H200)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C30(H30), C35(H35)
4.c Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C32(H32a,H32b,H32c), C33(H33a,H33b,
 H33c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c)
;
_shelx_res_checksum              7023
_ins_header
;
TITL RAM-43_scale in P2(1)/c 

REM P2(1)/c (#14 in standard setting)

CELL 1.54184  15.997741  12.827151  19.739328  90.0000  95.3795  90.0000

ZERR    4.00   0.000155   0.000127   0.000151   0.0000   0.0008   0.0000

LATT  1

SYMM -x, y+1/2,-z+1/2 

SFAC C H B N O Ge W

UNIT 152.00 144.00 4.00 24.00 8.00 4.00 4.00

TREF

HKLF 4

END
;
_olex2_submission_original_sample_id RAM-43
_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 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.719