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_7703824
_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 Fe I P4, Cl O4'
_chemical_formula_sum            'C36 H56 Cl Fe I O4 P4'
_chemical_formula_weight         894.88
_chemical_name_common            delta-[FeI{(S,S)-Me-DuPhos}2](ClO4)
_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             2019-08-23
_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            8
_cell_length_a                   11.23747(14)
_cell_length_b                   20.9195(3)
_cell_length_c                   33.7258(4)
_cell_measurement_reflns_used    36898
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6240
_cell_measurement_theta_min      3.1710
_cell_volume                     7928.34(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
  1 omega  -20.00   29.70   0.7000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6603  -99.0000 -180.0000 71

  2 omega -109.00  -55.10   0.7000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6603  178.0000 -120.0000 77

  3 omega -112.00  -57.40   0.7000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6603 -178.0000 -180.0000 78

  4 omega  -20.00  100.40   0.7000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9103   38.0000 -150.0000 172

  5 omega  -72.00   99.50   0.7000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9103  -19.0000 -150.0000 245

  6 omega  -70.00   15.40   0.7000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9103  -67.0000   48.2429 122
;
_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      0.0493685000
_diffrn_orient_matrix_UB_12      0.0022281000
_diffrn_orient_matrix_UB_13      0.0130209000
_diffrn_orient_matrix_UB_21      0.0213348000
_diffrn_orient_matrix_UB_22      -0.0298371000
_diffrn_orient_matrix_UB_23      -0.0070255000
_diffrn_orient_matrix_UB_31      0.0330383000
_diffrn_orient_matrix_UB_32      0.0159648000
_diffrn_orient_matrix_UB_33      -0.0149414000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            93611
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.103
_diffrn_reflns_theta_min         2.922
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.424
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             3680
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF-d8'
_exptl_crystal_size_max          0.2894
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.0625
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 6797 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         19581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0498P)^2^+11.1151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                17109
_reflns_number_total             19581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04821a2.cif
_cod_data_source_block           str1619
_cod_depositor_comments
'Adding full bibliography for 7703821--7703824.cif.'
_cod_database_code               7703824
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 D8 B F4 O P4 Fe'
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.683
_reflns_odcompleteness_completeness 99.71
_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: O2(0.51) O8(0.54) O9(0.49) O10(0.46)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C5(H5), C12(H12), C11(H11), C13(H13), C19(H19),
 C21(H21), C26(H26), C24(H24), C29(H29), C30(H30), C38(H38), C34(H34), C40(H40)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C8(H8A,H8B), C7(H7A,H7B), C10(H10A,H10B), C25(H25A,H25B),
 C39(H39A,H39B), C45(H45A,H45B), C54(H54A,H54B), C59(H59A,H59B), C58(H58A,H58B),
  C55(H55A,H55B), C66(H66A,H66B), C65(H65A,H65B), C74(H74A,H74B), C71(H71A,
 H71B), C72(H72A,H72B)
3.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C15(H15), C33(H33), C37(H37), C42(H42), C48(H48), C47(H47),
 C49(H49), C50(H50), C52(H52), C51(H51), C63(H63), C62(H62), C64(H64), C70(H70),
  C73(H73)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C31(H31A,H31B,
 H31C), C28(H28A,H28B,H28C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C43(H43A,
 H43B,H43C), C61(H61A,H61B,H61C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C),
 C53(H53A,H53B,H53C), C68(H68A,H68B,H68C), C67(H67A,H67B,H67C), C69(H69A,H69B,
 H69C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              86982
_olex2_date_sample_data_collection 2014-02-27
_olex2_submission_special_instructions 'No special instructions were received'