Syntheses, characterizations, and reactivities of new 1,4,7-trimethyl-l,4,7-triazacyclononane (Me3tacn) molybdenum and tungsten complexes
Zhang, Cai-Xia; Fang, Duo-Wen; Wang, Jun-Ling; Jia, Ai-Quan; Zhang, Qian-Feng; Inorganica Chimica Acta 507 (2020) 119599–; doi:10.1016/j.ica.2020.119599

data_1564861
_publ_section_title
;
 Syntheses, characterizations, and reactivities of new
 1,4,7-trimethyl-l,4,7-triazacyclononane (Me3tacn) molybdenum and tungsten
 complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119599
_journal_paper_doi               10.1016/j.ica.2020.119599
_journal_volume                  507
_journal_year                    2020
_chemical_formula_sum            'C14 H31 I N4 O4 S2 W'
_chemical_formula_weight         694.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                69.8019(12)
_cell_angle_beta                 88.2229(13)
_cell_angle_gamma                77.6266(12)
_cell_formula_units_Z            2
_cell_length_a                   8.4175(9)
_cell_length_b                   10.2748(12)
_cell_length_c                   14.4639(16)
_cell_measurement_reflns_used    3646
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.48
_cell_volume                     1145.5(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7265
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.408
_diffrn_reflns_theta_min         2.164
_exptl_absorpt_coefficient_mu    6.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_exptl_transmission_factor_max   0.397
_exptl_transmission_factor_min   0.278
_refine_diff_density_max         1.079
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0409P)^2^+0.2530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4543
_reflns_number_total             5043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5a.cif
_cod_data_source_block           P-1
_cod_database_code               1564861
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.352
_shelx_estimated_absorpt_t_max   0.459
_shelx_res_checksum              86331
_shelx_hkl_checksum              34929