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_7703823
_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_formula_moiety         'C36 H56 Fe I P4, I, H2 O'
_chemical_formula_sum            'C36 H58 Fe I2 O P4'
_chemical_formula_weight         940.35
_chemical_name_common            cappa-[FeI{(R,R)-Me-DuPhos}2]I2\^A.H2O
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-21
_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                 103.587(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3411(3)
_cell_length_b                   20.8867(4)
_cell_length_c                   17.3185(3)
_cell_measurement_reflns_used    33222
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.9840
_cell_measurement_theta_min      3.5150
_cell_volume                     3987.57(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_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
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -41.00  62.60   0.70   20.00    --  -11.13  57.00 120.00  148
  2  \w    -20.00  29.70   0.70   20.00    --  -11.13 -99.00-150.00   71
  3  \w    -20.00  29.70   0.70   20.00    --  -11.13 -99.00 -90.00   71
  4  \w    -14.00  87.50   0.70   20.00    --   12.06  37.00-180.00  145
  5  \w    -64.00  37.50   0.70   20.00    --   12.06 -37.00   0.00  145
  6  \w    -18.00  85.60   0.70   20.00    --   12.06  57.00  90.00  148
  7  \w    -67.00  45.00   0.70   20.00    --   12.06 -77.00 -30.00  160
  8  \w    -41.00  62.60   0.70   20.00    --  -11.13  57.00-180.00  148
  9  \w    -20.00  29.70   0.70   20.00    --  -11.13 -99.00-180.00   71
 10  \w    -70.00 -44.10   0.70   20.00    --  -11.13 127.00-179.45   37
 11  \w   -100.00 -55.90   0.70   20.00    --  -11.13 178.00 120.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0325972000
_diffrn_orient_matrix_UB_12      -0.0063827000
_diffrn_orient_matrix_UB_13      -0.0394738000
_diffrn_orient_matrix_UB_21      0.0057324000
_diffrn_orient_matrix_UB_22      -0.0333565000
_diffrn_orient_matrix_UB_23      0.0076763000
_diffrn_orient_matrix_UB_31      -0.0551745000
_diffrn_orient_matrix_UB_32      0.0003030000
_diffrn_orient_matrix_UB_33      0.0125735000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            70382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.000
_diffrn_reflns_theta_max         24.000
_diffrn_reflns_theta_min         2.850
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
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_colour            'dull light red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF-d8'
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 5583 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12484
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0285P)^2^+2.0210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11976
_reflns_number_total             12484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04821a2.cif
_cod_data_source_block           str1832
_cod_depositor_comments
'Adding full bibliography for 7703821--7703824.cif.'
_cod_original_cell_volume        3987.58(14)
_cod_database_code               7703823
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H I Fe P'
_reflns_odcompleteness_completeness 99.80
_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, All O(H,H) groups
2. Others
 Fixed Sof: I3(0.6) I4(0.805) I5(0.195) I6(0.4)
3.a Free rotating group:
 O1(H1A,H1B), O0AA(H0AA,H0AB)
3.b Ternary CH refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C20(H20), C25(H25), C31(H31), C29(H29), C39(H39), C51(H51), C57(H57)
3.c Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C34(H34A,H34B), C37(H37A,
 H37B), C43(H43A,H43B), C42(H42A,H42B), C45(H45A,H45B), C55(H55A,H55B),
 C64(H64A,H64B), C63(H63A,H63B), C62(H62A,H62B), C60(H60A,H60B), C59(H59A,H59B),
  C61(H61A,H61B), C66(H66A,H66B)
3.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C19(H19), C21(H21), C24(H24), C36(H36), C41(H41), C46(H46),
 C47(H47), C48(H48), C53(H53), C54(H54), C58(H58), C68(H68), C69(H69), C71(H71),
  C72(H72)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C), C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C),
 C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C67(H67A,H67B,H67C), C65(H65A,H65B,
 H65C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              74174
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.832