Synthesis and structural characterization of metal complexes with macrocyclic tetracarbene ligands
Fei, Fan; Lu, Taotao; Chen, Xue-tai; Xue, Ziling Ben; New J. Chem. 41 (2017) 13442–13453; doi:10.1039/C7NJ02485A

data_7056650
_publ_section_title
;
 Synthesis and structural characterization of metal complexes with
 macrocyclic tetracarbene ligands
;
_journal_issue                   22
_journal_name_full               'New J. Chem.'
_journal_page_first              13442
_journal_page_last               13453
_journal_paper_doi               10.1039/C7NJ02485A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C264 H288 Ag12 F72 N48 P12'
_chemical_formula_weight         7167.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.573(2)
_cell_length_b                   43.500(3)
_cell_length_c                   45.318(3)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.58
_cell_measurement_theta_min      2.38
_cell_volume                     62241(7)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            114889
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         0.915
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.7681
_exptl_absorpt_correction_T_min  0.7498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.320
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_platon_squeeze_details
;
;
_refine_diff_density_max         1.577
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_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         13704
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_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1189
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_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^)+(0.1466P)^2^+1915.3652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2627
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_reflns_number_gt                10279
_reflns_number_total             13704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02485a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        62242(7)
_cod_database_code               7056650
_shelx_estimated_absorpt_t_min   0.750
_shelx_estimated_absorpt_t_max   0.768
_shelxl_version_number           2014/6
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