Molybdenum dinitrogen complex supported by a cyclohexane-based triphosphine ligand and dmpm.
Weyrich, Thomas; Krahmer, Jan; Engesser, Tobias A.; Näther, Christian; Tuczek, Felix; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6019–6025; doi:10.1039/c8dt04738c

data_7048822
_publ_section_title
;
 Molybdenum dinitrogen complex supported by a cyclohexane-based
 triphosphine ligand and dmpm.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6019
_journal_page_last               6025
_journal_paper_doi               10.1039/c8dt04738c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C42 H39 P3'
_chemical_formula_weight         636.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-11-30 deposited with the CCDC.
2019-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7012(2)
_cell_length_b                   23.6772(6)
_cell_length_c                   13.8942(4)
_cell_measurement_reflns_used    23836
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.005
_cell_measurement_theta_min      1.699
_cell_volume                     3520.44(15)
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23836
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.005
_diffrn_reflns_theta_min         1.699
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 3130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7671
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0494P)^2^+0.4162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7081
_reflns_number_total             7671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04738c2.cif
_cod_data_source_block           felix138
_cod_depositor_comments
'Adding full bibliography for 7048821--7048822.cif.'
_cod_database_code               7048822
_shelxl_version_number           2014-3
_shelx_res_checksum              43525