Bulky 1,1'-bisphosphanoferrocenes and their coordination behaviour towards Cu(i).
Dey, Subhayan; Buzsáki, Daniel; Bruhn, Clemens; Kelemen, Zsolt; Pietschnig, Rudolf; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6668–6681; doi:10.1039/d0dt00941e

data_7704212
_publ_section_title
;
 Bulky 1,1'-bisphosphanoferrocenes and their coordination behaviour
 towards Cu(i).
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6668
_journal_page_last               6681
_journal_paper_doi               10.1039/d0dt00941e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H46 Cu Fe N2 P2, B F4'
_chemical_formula_sum            'C44 H46 B Cu F4 Fe N2 P2'
_chemical_formula_weight         870.97
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-27 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.048(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8168(4)
_cell_length_b                   19.2843(5)
_cell_length_c                   16.9754(5)
_cell_measurement_reflns_used    29358
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      1.21
_cell_volume                     4164.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 140 frames, detector distance = 120 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2, 0.6 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17948
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.605
_diffrn_source                   'Genix Mo HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.8751
_exptl_absorpt_correction_T_min  0.5381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.689
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+8.1674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6832
_reflns_number_total             7743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00941e2.cif
_cod_data_source_block           i2964
_cod_depositor_comments
'Adding full bibliography for 7704207--7704214.cif.'
_cod_database_code               7704212
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H42A,H42B,H42C} of C42, {H38A,H38B,H38C} of C38, {H31A,
  H31B,H31C} of C31, {H30A,H30B,H30C} of C30, {H40A,H40B,H40C} of C40, {H39A,
  H39B,H39C} of C39, {H29A,H29B,H29C} of C29
 At 1.5 times of:
  {H46A,H46B,H46C} of C46, {H44A,H44B,H44C} of C44
2. Rigid body (RIGU) restrains
 C45
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
3. Others
 Fixed Sof: C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C44(0.5) H44A(0.5)
 H44B(0.5) H44C(0.5) C45(0.5) C43(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C25(H25), C27(H27), C34(H34), C36(H36)
4.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C46(H46A,
 H46B,H46C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              68192
_olex2_submission_special_instructions 'No special instructions were received'