Merging metal-ligand cooperation and redox promoted strategy for tailored synthesis of alkylated 9<i>H</i>-fluorenes.
Samanta, Arup; Phukan, Hirak Jyoti; Tripathi, Ujjwal Kumar; Srimani, Dipankar; Chemical communications (Cambridge, England) 61 (2025) 12582–12585; doi:10.1039/d5cc02867a

data_7134821
_publ_section_title
;
 Merging metal-ligand cooperation and redox promoted strategy for tailored
 synthesis of alkylated 9<i>H</i>-fluorenes.
;
_journal_issue                   67
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12582
_journal_page_last               12585
_journal_paper_doi               10.1039/d5cc02867a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C13 H13 Br2 N3 O Zn'
_chemical_formula_weight         452.45
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-05-20 deposited with the CCDC.	2025-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.091(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4493(10)
_cell_length_b                   15.5797(12)
_cell_length_c                   7.6731(6)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.61
_cell_volume                     1544.8(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            34268
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.048
_exptl_absorpt_coefficient_mu    6.760
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2505
_reflns_number_total             2696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02867a2.cif
_cod_data_source_block           ZN_8_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7134820--7134825.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7134821
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              28506
_shelx_hkl_checksum              90382