Configurational landscape of chiral iron(ii) bis(phosphane) complexes.
Estevan, Francisco; Feliz, Marta; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4528–4538; doi:10.1039/c9dt04821a

data_7703822
_publ_section_title
;
 Configurational landscape of chiral iron(ii) bis(phosphane) complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4528
_journal_page_last               4538
_journal_paper_doi               10.1039/c9dt04821a
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C36 H56 Cl Fe P4, B F4'
_chemical_formula_sum            'C36 H56 B Cl F4 Fe P4'
_chemical_formula_weight         790.79
_chemical_name_common            '[FeCl{(R,R)-Me-DuPhos}2](BF4)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2020-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8107(3)
_cell_length_b                   16.8676(4)
_cell_length_c                   15.5365(3)
_cell_measurement_reflns_used    17631
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5710
_cell_measurement_theta_min      3.2120
_cell_volume                     3881.34(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -46.00   24.00   0.7000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   80.0000  136.0000 100

  2 omega -100.00  -55.90   0.7000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000  120.0000 63

  3 omega  -20.00   29.70   0.7000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000  -30.0000 71

  4 omega  -20.00   29.70   0.7000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000  150.0000 71

  5 omega   34.00   99.10   0.7000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628 -178.0000  -60.0000 93

  6 omega  -14.00   87.50   0.7000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628   37.0000   90.0000 145

  7 omega   35.00   81.20   0.7000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628  178.0000   90.0000 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0436310000
_diffrn_orient_matrix_UB_12      -0.0089887000
_diffrn_orient_matrix_UB_13      -0.0160604000
_diffrn_orient_matrix_UB_21      -0.0171894000
_diffrn_orient_matrix_UB_22      -0.0349345000
_diffrn_orient_matrix_UB_23      -0.0194453000
_diffrn_orient_matrix_UB_31      -0.0096349000
_diffrn_orient_matrix_UB_32      0.0216353000
_diffrn_orient_matrix_UB_33      -0.0380587000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.998
_diffrn_reflns_theta_max         23.998
_diffrn_reflns_theta_min         2.779
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CD2Cl2'
_exptl_crystal_size_max          0.3475
_exptl_crystal_size_mid          0.2515
_exptl_crystal_size_min          0.1435
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2405 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+3.6528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5728
_reflns_number_total             6074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04821a2.cif
_cod_data_source_block           str1816
_cod_depositor_comments
'Adding full bibliography for 7703821--7703824.cif.'
_cod_original_cell_volume        3881.34(15)
_cod_database_code               7703822
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H96 P12 B F4 I Fe '
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F1(0.61) F2(0.59) F3(0.63) F4(0.41) F5(0.7) F0AA(0.37) F6(0.3)
 F7(0.39)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C16(H16), C19(H19), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B),
 C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C2AA(H2AA), C4(H4), C15(H15), C28(H28), C31(H31), C29(H29), C30(H30)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              7958
_olex2_submission_special_instructions 'No special instructions were received'