Salan group 13 complexes ‒ structural study and lactide polymerisation
Beament, James; Mahon, Mary F.; Buchard, Antoine; Jones, Matthew D.; New J. Chem. 41 (2017) 2198–; doi:10.1039/C6NJ03844A

data_7055996
_publ_section_title
;
 Salan group 13 complexes -- structural study and lactide polymerisation
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              2198
_journal_paper_doi               10.1039/C6NJ03844A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C34 H54 Cl Ga N2 O2'
_chemical_formula_sum            'C40 H68 Cl Ga N2 O2'
_chemical_formula_weight         714.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-10-18 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3759(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.9563(6)
_cell_length_b                   14.0324(2)
_cell_length_c                   17.9476(2)
_cell_measurement_reflns_used    24351
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.9630
_cell_measurement_theta_min      3.4060
_cell_volume                     8136.9(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46467
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.437
_diffrn_reflns_theta_min         2.735
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81232
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       cube
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8157
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0575P)^2^+15.1669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7494
_reflns_number_total             8157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03844a2.cif
_cod_data_source_block           Ga_2_Cl
_cod_depositor_comments
'Adding full bibliography for 7055992--7055999.cif.'
_cod_database_code               7055996
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.718
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C11 \\sim C13A-C11 \\sim C13-C11 \\sim C14A-C11 \\sim C14-C11 \\sim
C12A-C11 \\sim C30A-C27
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C12A \\sim C13A \\sim C14A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
C28 \\sim C29 \\sim C30 \\sim C28A \\sim C29A \\sim C30A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C12(0.8) H12A(0.8) H12B(0.8) H12C(0.8) C13(0.8) H13A(0.8)
 H13B(0.8) H13C(0.8) C14(0.8) H14A(0.8) H14B(0.8) H14C(0.8) C28(0.6) H28A(0.6)
 H28B(0.6) H28C(0.6) C29(0.6) H29A(0.6) H29B(0.6) H29C(0.6) C30(0.6) H30A(0.6)
 H30B(0.6) H30C(0.6) C12A(0.2) H12D(0.2) H12E(0.2) H12F(0.2) C13A(0.2)
 H13D(0.2) H13E(0.2) H13F(0.2) C14A(0.2) H14D(0.2) H14E(0.2) H14F(0.2)
 C28A(0.4) H28D(0.4) H28E(0.4) H28F(0.4) C29A(0.4) H29D(0.4) H29E(0.4)
 H29F(0.4) C30A(0.4) H30D(0.4) H30E(0.4) H30F(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C22(H22), C24(H24)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C12A(H12D,H12E,H12F),
 C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C28A(H28D,H28E,H28F), C29A(H29D,
 H29E,H29F), C30A(H30D,H30E,H30F)
;
_shelx_fab_checksum              446
_shelx_shelxl_version_number     2014/7
_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 1.594
_oxdiff_exptl_absorpt_empirical_full_min 0.700