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_7134822
_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            'C14 H18 Br2 N4 O S Zn'
_chemical_formula_weight         515.57
_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   geom
_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                 98.261(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9413(6)
_cell_length_b                   13.4749(8)
_cell_length_c                   14.3357(8)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.27
_cell_measurement_theta_min      2.56
_cell_volume                     1900.46(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44533
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.070
_exptl_absorpt_coefficient_mu    5.614
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_refine_diff_density_max         1.723
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.7398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2424
_reflns_number_total             3338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02867a2.cif
_cod_data_source_block           Zn7_2_0m_a
_cod_depositor_comments
'Adding full bibliography for 7134820--7134825.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7134822
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              16158
_shelx_hkl_checksum              49427