A transition metal-gallium cluster formed via insertion of "GaI".
Blundell, Toby J.; Taylor, Laurence J.; Valentine, Andrew J.; Lewis, William; Blake, Alexander J.; McMaster, Jonathan; Kays, Deborah L.; Chemical communications (Cambridge, England) 56 (2020) 8139–8142; doi:10.1039/d0cc03559a

data_7126688
_publ_section_title
;
 A transition metal-gallium cluster formed via insertion of
 &quot;GaI&quot;.
;
_journal_issue                   58
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8139
_journal_page_last               8142
_journal_paper_doi               10.1039/d0cc03559a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C28 H33 Co1 Ga3 I5'
_chemical_formula_sum            'C28 H33 Co Ga3 I5'
_chemical_formula_weight         1272.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Wed Apr 02 09:20:50 2014'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_audit_update_record
;
2020-05-18 deposited with the CCDC.	2020-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   16.6877(4)
_cell_length_b                   17.7466(4)
_cell_length_c                   24.3929(6)
_cell_measurement_reflns_used    27565
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.1860
_cell_measurement_theta_min      3.2040
_cell_volume                     7224.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -41.00  -14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  137.0000   28.0000 27

  2 omega  -94.00  -13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  150.0000 81

  3 omega -111.00  -19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  -90.0000 92

  4 omega -112.00   -7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -77.0000   30.0000 105

  5 omega   89.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   38.0000   60.0000 27

  6 omega    3.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -99.0000  150.0000 44

  7 omega   30.00   57.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -38.0000 -120.0000 27

  8 omega   48.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000  -90.0000 50

  9 omega   57.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -95.0000  120.0000 52

 10 omega   35.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000   30.0000 63

 11 omega   25.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -95.0000  -60.0000 79

 12 omega   60.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   15.0000  -90.0000 115

 13 omega   66.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000  -60.0000 31

 14 omega   48.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -30.0000   60.0000 38

 15 omega   60.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000   90.0000 32

 16 omega   45.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000 -180.0000 46

 17 omega  152.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  125.0000  120.0000 25

 18 omega   32.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -30.0000  -30.0000 55

 19 omega  115.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  125.0000  120.0000 27

 20 omega  138.00  174.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  125.0000 -180.0000 36

 21 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -95.0000 -150.0000 79

 22 omega   91.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087 -125.0000   90.0000 28

 23 omega   88.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   30.0000  -30.0000 90

 24 omega   12.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   77.0000  -30.0000 105

 25 omega    1.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -99.0000   30.0000 82

 26 omega   17.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   57.0000 -180.0000 96

 27 omega  -27.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -57.0000 -150.0000 97

 28 omega   12.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   77.0000 -120.0000 105

 29 omega   21.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   38.0000  120.0000 95

 30 omega   60.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   15.0000  120.0000 118

 31 omega   78.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   61.0000  -30.0000 97

 32 omega   74.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   77.0000  120.0000 104

 33 omega   78.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   61.0000  -90.0000 98

 34 omega   82.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   45.0000 -180.0000 95

 35 omega   78.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   61.0000    0.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0044718000
_diffrn_orient_matrix_UB_12      -0.0013083000
_diffrn_orient_matrix_UB_13      -0.0631033000
_diffrn_orient_matrix_UB_21      0.0672134000
_diffrn_orient_matrix_UB_22      -0.0593319000
_diffrn_orient_matrix_UB_23      0.0029075000
_diffrn_orient_matrix_UB_31      -0.0631354000
_diffrn_orient_matrix_UB_32      -0.0632926000
_diffrn_orient_matrix_UB_33      -0.0014267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2880
_diffrn_reflns_av_unetI/netI     0.1396
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            95072
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.580
_diffrn_reflns_theta_min         4.063
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.835
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.048
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    2.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.2977
_exptl_crystal_size_mid          0.2711
_exptl_crystal_size_min          0.0167
_refine_diff_density_max         6.599
_refine_diff_density_min         -3.064
_refine_diff_density_rms         0.697
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.777
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         6238
_refine_ls_number_restraints     1600
_refine_ls_restrained_S_all      2.473
_refine_ls_R_factor_all          0.2575
_refine_ls_R_factor_gt           0.2497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5893
_refine_ls_wR_factor_ref         0.5981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5294
_reflns_number_total             6238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03559a2.cif
_cod_data_source_block           gatble
_cod_depositor_comments
'Adding full bibliography for 7126685--7126689.cif.'
_cod_original_cell_volume        7223.9(3)
_cod_original_sg_symbol_H-M      'P c a m'
_cod_database_code               7126688
_nottingham_internal_coll_name   GATBLE
_nottingham_internal_coll_number 13431
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '5.0000, 20.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxtb
_nottingham_internal_coll_date   01/04/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 02/04/2014
_nottingham_internal_process_user pcxtb
_nottingham_internal_solution_date 15/06/2015
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 15/06/2015
_nottingham_internal_refinement_user pcxtb
_nottingham_internal_self_archive_date 16/06/2015
_nottingham_internal_self_validation_date 15/06/2015
_nottingham_internal_self_validation_user pcxtb
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C28 H33 Co Ga3 I5'
_cell_oxdiff_angle_alpha         90.002(2)
_cell_oxdiff_angle_beta          90.0311(19)
_cell_oxdiff_angle_gamma         90.0163(19)
_cell_oxdiff_length_a            16.6865(4)
_cell_oxdiff_length_b            17.7555(4)
_cell_oxdiff_length_c            24.3823(6)
_cell_oxdiff_measurement_reflns_used 27567
_cell_oxdiff_volume              7223.9(3)
_reflns_odcompleteness_completeness 99.90
_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. Restrained distances
 C8-C7 \\sim C7-C12
 with sigma of 0.02
 C9-C8 \\sim C12-C11
 with sigma of 0.02
 C11-C10 \\sim C9-C10
 with sigma of 0.02
 C17-C12 \\sim C16-C11 \\sim C15-C10 \\sim C9-C14 \\sim C8-C13
 with sigma of 0.02
3. Restrained planarity
 C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17
 with sigma of 0.1
 C6, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma of 0.1
 C1, C2, C3, C4, C5, C6, C7, C18
 with sigma of 0.1
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C18A
 with sigma of 0.1
 C18A, C19A, C20A, C21A, C22A, C23A, C28A, C24A, C25A, C26A, C27A, C6A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Same fragment restrains
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, Co4, Ga1, Ga2, Ga3, I1,
I2, I3, I4, I5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A,
C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A,
C28A, Co4A, Ga1A, Ga2A, Ga3A, I1A, I2A, I3A, I4A, I5A}
7. Others
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(C8A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(C12A)=Sof(C13A)=
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(C19A)=
 Sof(C20A)=Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(Co4A)=Sof(Ga1A)=Sof(Ga2A)=Sof(Ga3A)=Sof(I1A)=
 Sof(I2A)=Sof(I3A)=Sof(I4A)=Sof(I5A)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(C7)=Sof(C8)=Sof(C9)=Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(Co4)=Sof(Ga1)=Sof(Ga2)=Sof(Ga3)=
 Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=Sof(I5)=FVAR(1)
8.a Me refined with riding coordinates:
 C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F), C16A(H16D,
 H16E,H16F), C17A(H17D,H17E,H17F), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C3A(H3A), C4A(H4A), C5A(H5A)
8.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              23338
_shelx_hkl_checksum              61028
_olex2_exptl_crystal_mounting_method 'mounted in fomblin film on micromount'
_olex2_submission_special_instructions 'No special instructions were received'