Synthesis and characterization of M(ii) (M = Mn, Fe and Co) azafulvene complexes and their X3(-) derivatives.
Matson, Ellen M.; Park, Yun Ji; Bertke, Jeffery A.; Fout, Alison R.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10377–10384; doi:10.1039/c5dt00985e

data_7035159
_publ_section_title
;
 Synthesis and characterization of M(ii) (M = Mn, Fe and Co) azafulvene
 complexes and their X3(-) derivatives.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10377
_journal_page_last               10384
_journal_paper_doi               10.1039/c5dt00985e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C37 H51 Co F3 N7 O3 S, C F3 O3 S, C4 H8 O'
_chemical_formula_sum            'C42 H59 Co F6 N7 O7 S2'
_chemical_formula_weight         1011.01
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-04-16 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.718(2)
_cell_length_b                   16.199(3)
_cell_length_c                   27.605(6)
_cell_measurement_reflns_used    1308
_cell_measurement_temperature    176(2)
_cell_measurement_theta_max      23.35
_cell_measurement_theta_min      2.39
_cell_volume                     4792.8(16)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
;
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      176(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm79b
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            10200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.950
_diffrn_reflns_theta_min         1.458
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.9310
_exptl_absorpt_correction_T_min  0.8869
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2116
_exptl_crystal_id                cm79b
_exptl_crystal_preparation
;
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0, -1, 5) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 3282 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.029(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         10200
_refine_ls_number_restraints     617
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0398P)^2^+0.1124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                8543
_reflns_number_total             10200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00985e2.cif
_cod_data_source_block           cm79bas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035158--7035164.cif.
;
_cod_original_cell_volume        4792.8(17)
_cod_database_code               7035159
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.049) H6(0.048) H7(0.049) H20A(0.037) H20B(0.037) H30A(0.037)
 H30B(0.037) H40A(0.035) H40B(0.035) H22A(0.043) H23A(0.043) H25A(0.036)
 H32A(0.047) H33A(0.043) H35A(0.034) H42A(0.047) H43A(0.043) H45A(0.033)
 H51A(0.037) H52A(0.047) H52B(0.047) H53A(0.055) H53B(0.055) H54A(0.058)
 H54B(0.058) H55A(0.056) H55B(0.056) H56A(0.052) H56B(0.052) H61A(0.04)
 H62A(0.045) H62B(0.045) H63A(0.056) H63B(0.056) H64A(0.061) H64B(0.061)
 H65A(0.057) H65B(0.057) H66A(0.048) H66B(0.048) H71(0.038) H72A(0.049)
 H72B(0.049) H73A(0.062) H73B(0.062) H74A(0.061) H74B(0.061) H75A(0.061)
 H75B(0.061) H76A(0.049) H76B(0.049) H71B(0.041) H72C(0.048) H72D(0.048)
 H73C(0.057) H73D(0.057) H74C(0.062) H74D(0.062) H75C(0.056) H75D(0.056)
 H76C(0.05) H76D(0.05) H81A(0.068) H81B(0.068) H82A(0.079) H82B(0.079)
 H83A(0.08) H83B(0.08) H84A(0.079) H84B(0.079) H81C(0.074) H81D(0.074)
 H82C(0.079) H82D(0.079) H83C(0.091) H83D(0.091) H84C(0.086) H84D(0.086)
 Fixed X: H20A(-0.4517) H20B(-0.5332) H30A(-0.4266) H30B(-0.508) H40A(-0.453)
 H40B(-0.526) H22A(-0.4686) H23A(-0.2649) H25A(-0.0053) H32A(-0.3906) H33A(-
 0.178) H35A(-0.0073) H42A(-0.4448) H43A(-0.2371) H45A(0.0045) H51A(0.1806)
 H52A(0.1412) H52B(0.1597) H53A(0.3681) H53B(0.3508) H54A(0.3329) H54B(0.4593)
 H55A(0.346) H55B(0.3666) H56A(0.1387) H56B(0.159) H61A(0.147) H62A(0.1611)
 H62B(0.0713) H63A(0.2446) H63B(0.2545) H64A(0.4504) H64B(0.4011) H65A(0.4715)
 H65B(0.3826) H66A(0.2882) H66B(0.2979) H71(0.1959) H72A(0.1582) H72B(0.2017)
 H73A(0.3736) H73B(0.3945) H74A(0.4478) H74B(0.3136) H75A(0.3573) H75B(0.3159)
 H76A(0.1201) H76B(0.1419) H71B(0.1973) H72C(0.1756) H72D(0.151) H73C(0.3608)
 H73D(0.3814) H74C(0.4659) H74D(0.3426) H75C(0.3705) H75D(0.3439) H76C(0.1393)
 H76D(0.1606) H81A(0.7302) H81B(0.7467) H82A(0.6577) H82B(0.6942) H83A(0.8668)
 H83B(0.8178) H84A(0.9238) H84B(1.0202) H81C(0.7835) H81D(0.7508) H82C(0.6566)
 H82D(0.6626) H83C(0.7893) H83D(0.8188) H84C(1.0051) H84D(0.9327)
 Fixed Y: H20A(0.3123) H20B(0.3298) H30A(0.523) H30B(0.447) H40A(0.4233)
 H40B(0.4874) H22A(0.173) H23A(0.113) H25A(0.2608) H32A(0.4713) H33A(0.4271)
 H35A(0.3426) H42A(0.6239) H43A(0.6957) H45A(0.5598) H51A(0.1915) H52A(0.075)
 H52B(0.1724) H53A(0.1637) H53B(0.1005) H54A(-0.0106) H54B(0.038) H55A(0.0056)
 H55B(0.103) H56A(0.0169) H56B(0.0806) H61A(0.2599) H62A(0.237) H62B(0.1862)
 H63A(0.125) H63B(0.1085) H64A(0.153) H64B(0.2157) H65A(0.2923) H65B(0.2413)
 H66A(0.3696) H66B(0.3552) H71(0.6316) H72A(0.7905) H72B(0.709) H73A(0.7989)
 H73B(0.7103) H74A(0.8126) H74B(0.8549) H75A(0.6958) H75B(0.7763) H76A(0.7768)
 H76B(0.6876) H71B(0.6332) H72C(0.7485) H72D(0.8076) H73C(0.8221) H73D(0.7243)
 H74C(0.7783) H74D(0.8305) H75C(0.6571) H75D(0.7214) H76C(0.7421) H76D(0.6444)
 H81A(0.2272) H81B(0.1903) H82A(0.0781) H82B(0.1033) H83A(0.0323) H83B(-0.0051)
 H84A(0.0932) H84B(0.0812) H81C(0.2145) H81D(0.2368) H82C(0.1169) H82D(0.1051)
 H83C(0.0021) H83D(0.0366) H84C(0.0633) H84D(0.0932)
 Fixed Z: H20A(0.8254) H20B(0.8731) H30A(0.8225) H30B(0.8027) H40A(0.932)
 H40B(0.8978) H22A(0.9116) H23A(0.9375) H25A(0.905) H32A(0.7087) H33A(0.6806)
 H35A(0.7919) H42A(0.953) H43A(0.9537) H45A(0.8945) H51A(0.9173) H52A(0.9944)
 H52B(1.0016) H53A(0.9734) H53B(1.0175) H54A(0.9641) H54B(0.952) H55A(0.8801)
 H55B(0.8856) H56A(0.9064) H56B(0.8626) H61A(0.7685) H62A(0.6657) H62B(0.7012)
 H63A(0.7395) H63B(0.6824) H64A(0.7145) H64B(0.6739) H65A(0.7407) H65B(0.7764)
 H66A(0.761) H66B(0.7036) H71(0.9095) H72A(0.9528) H72B(0.9808) H73A(0.9654)
 H73B(0.941) H74A(0.8852) H74B(0.891) H75A(0.8495) H75B(0.8198) H76A(0.858)
 H76B(0.8345) H71B(0.9285) H72C(0.9803) H72D(0.9347) H73C(0.9574) H73D(0.9554)
 H74C(0.886) H74D(0.875) H75C(0.8652) H75D(0.8225) H76C(0.8493) H76D(0.8444)
 H81A(0.7602) H81B(0.8141) H82A(0.783) H82B(0.7284) H83A(0.732) H83B(0.7826)
 H84A(0.8275) H84B(0.7829) H81C(0.7444) H81D(0.7998) H82C(0.811) H82D(0.7531)
 H83C(0.7696) H83D(0.823) H84C(0.7825) H84D(0.734)
;