Poly(ferrocenylene iminoborane): an inorganic–organic hybrid polymer comprising a backbone of moderately interacting ferrocenes
Zeh, Vivien; Schneider, Johannes Stephan; Bachmann, Jonas; Krummenacher, Ivo; Braunschweig, Holger; Helten, Holger; Chemical Communications  (2023) –; doi:10.1039/D3CC03523A

data_7132267
_publ_section_title
;
 Poly(ferrocenylene iminoborane): an inorganic--organic hybrid polymer
 comprising a backbone of moderately interacting ferrocenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03523A
_journal_year                    2023
_chemical_formula_moiety         'C48 H50 B2 Fe3 N2'
_chemical_formula_sum            'C48 H50 B2 Fe3 N2'
_chemical_formula_weight         844.07
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-07-04
_audit_creation_method           'CIF-fill 1.4k (K.Radacki, 2005-23)'
_audit_update_record
;
2023-07-19 deposited with the CCDC.	2023-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.11(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.066(11)
_cell_length_b                   7.861(4)
_cell_length_c                   24.097(13)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.65
_cell_volume                     3975(4)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 2011.8 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40B (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            Apex2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
;
 Sparks R.A., Computational Crystallography p1-18 (Clarendon Press, 1982)
;
_diffrn_orient_matrix_UB_11      0.0207803
_diffrn_orient_matrix_UB_12      -0.0518488
_diffrn_orient_matrix_UB_13      -0.0318262
_diffrn_orient_matrix_UB_21      -0.0333791
_diffrn_orient_matrix_UB_22      -0.0911975
_diffrn_orient_matrix_UB_23      -0.0033120
_diffrn_orient_matrix_UB_31      -0.0271282
_diffrn_orient_matrix_UB_32      0.0724951
_diffrn_orient_matrix_UB_33      -0.0269287
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57228
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.231
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Nonius FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_preparation
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 700).
;
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.154
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0836
_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^)+(0.0531P)^2^+31.4465P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6257
_reflns_number_total             7838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03523a2.cif
_cod_data_source_block           cmpd_6
_cod_original_cell_volume        3975(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7132267
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
 Incident beam scaling, empirical absorption correction using spherical 
 harmonics, and outlier rejection was employed as implemented in SADABS. 
 Additional spherical absorption correction with mu*r value set to 0.2 was 
 applied.
;
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.847
_shelx_res_checksum              24654
_shelx_hkl_checksum              42479