New Fe(III)(cyclam) Complexes Bearing Axially Boundgeminal-Diethynylethenes
Cao, Zhi; Fanwick, Phillip E.; Forrest, William P.; Gao, Yang; Ren, Tong; Organometallics 32 (2013) 4684–; doi:10.1021/om400683d

data_4081400
_publ_section_title
;
 New Fe(III)(cyclam) Complexes Bearing Axially
 Boundgeminal-Diethynylethenes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4684
_journal_paper_doi               10.1021/om400683d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C38 H46 Fe1 N4,C1 F3 O3 S1'
_chemical_formula_sum            'C39 H46 F3 Fe N4 O3 S'
_chemical_formula_weight         763.71
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.162(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2898(4)
_cell_length_b                   11.5783(5)
_cell_length_c                   26.8427(10)
_cell_measurement_reflns_used    36926
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.248
_cell_measurement_theta_min      3.301
_cell_volume                     3809.5(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'DIRDIF/PATTY (Burskens, et. al,. 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36926
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.248
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    4.158
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       needle
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0956P)^2^+3.4042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5029
_reflns_number_total             6826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400683d_si_002.cif
_cod_data_source_block           ZGEM1
_cod_database_code               4081400
_shelx_estimated_absorpt_t_min   0.490
_shelx_estimated_absorpt_t_max   0.851
_shelxl_version_number           2013-3
_shelx_res_checksum              71073
_shelx_hkl_checksum              53579