Insights on the electron-donating and withdrawing effect of the functional groups on mechanochemical dehydrochlorination reactions
Marti-Rujas, javier; Guo, Fang; Wang, Zhen; Zhang, Jinjing; Li, Hai Tao; Famulari, Antonino; Dalton Trans.  (2017) –; doi:10.1039/C7DT01710C

data_7043425
_publ_section_title
;
 Insights on the electron-donating and withdrawing effect of the
 functional groups on mechanochemical dehydrochlorination reactions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01710C
_journal_year                    2017
_chemical_formula_moiety         'Cl4 Co, C34 H30 F12 N2'
_chemical_formula_sum            'C34 H30 Cl4 Co F12 N2'
_chemical_formula_weight         895.33
_chemical_name_systematic
;
 ? 
;
_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             2017-05-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-10 deposited with the CCDC.
2017-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.075(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.184(5)
_cell_length_b                   9.121(3)
_cell_length_c                   28.925(10)
_cell_measurement_reflns_used    5492
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      25.191
_cell_measurement_theta_min      2.342
_cell_volume                     3983(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21381
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.056
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         7750
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0411P)^2^+6.6739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5509
_reflns_number_total             7750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01710c2.cif
_cod_data_source_block           4
_cod_database_code               7043425
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
F7 \\sim F7A \\sim F8 \\sim F8A \\sim F9 \\sim F9A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
F10 \\sim F10A \\sim F11 \\sim F11A \\sim F12 \\sim F12A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
3. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Fixed Sof: F10(0.5) F10A(0.5) F11(0.5) F11A(0.5) F12(0.5) F12A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C19(H19A,H19B), C11(H11A,H11B), C3(H3A,H3B), C1(H1A,H1B),
 C27(H27A,H27B)
4.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C33(H33), C21(H21), C9(H9), C5(H5), C17(H17), C13(H13), C8(H8),
 C16(H16), C32(H32), C6(H6), C30(H30), C14(H14), C25(H25), C24(H24), C22(H22)
;
_olex2_submission_special_instructions 'No special instructions were received'